CN104892416A - 2-Ethylhexyl acrylate waste oil recovery technology - Google Patents
2-Ethylhexyl acrylate waste oil recovery technology Download PDFInfo
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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
- C07C51/377—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by splitting-off hydrogen or functional groups; by hydrogenolysis of functional groups
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
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- 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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- 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
- C07C67/60—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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Abstract
The invention discloses a 2-ethylhexyl acrylate waste oil recovery technology including six steps of depolymerization, depolymerized material esterification, back distillation, neutralization, low boiling fraction removal and high boiling fraction removal. By addition of the back distillation step between the esterification and neutralization steps, 2-ethylhexyl acrylate and a polymerization inhibitor added in the depolymerization and esterification steps are separated, other high boiling point impurities can also be isolated at the same time, and the addition amount and proportion selected control of the polymerization inhibitor in the low boiling fraction removal step can be facilitated.
Description
Technical field
The present invention relates to acrylate waste oil and reclaim field, be specifically related to a kind of ethyl acrylate waste oil recovery process.
Background technology
Ethyl acrylate is a kind of important synthetic intermediate, is also the monomer of synthesising macromolecule copolymer, is widely used in rubber, medicine, leather, papermaking, tackiness agent and coating industry.The waste oil amount produced in the production process of current vinylformic acid and esters of acrylic acid increases, and needs to process accordingly.Main component in ethyl acrylate waste oil is ethyl acrylate, vinylformic acid, isooctyl alcohol, water and methoxy acrylic acid-2-ethylhexyl etc.In prior art, the recovery of ethyl acrylate mainly comprises cracking, esterification, de-light and de-heavy four operations.Disclose the retrieving arrangement of a kind of vinylformic acid and esters of acrylic acid waste oil in Chinese patent 200820214814.5, the cracking wherein mentioned, esterification, neutralization, washing, de-light, de-weight, this technique is applicable to the recovery of butyl acrylate and Octyl acrylate; Disclose the manufacture method of one (methyl) acrylate in CN101239909B, comprise esterification, washing except the operation such as acid catalyst, neutralization.
Ethyl acrylate contains unstable carbon-carbon double bond, and be easy to addition reaction occurs in production storage process, light, heat and superoxide all can accelerate its polymerization, usually needs to use stopper to prevent the carrying out of polymerization.Different types of stopper mechanism of action differs, and have the technical scheme adopting single stopper in prior art, its polymerization inhibition effect is undesirable.In addition, stopper consumption too much can affect polymerization inhibition effect.In prior art, after esterification, vinylformic acid in liquid caustic soda He excessive can be adopted, after by neutralization produce oil reservoir directly rotate de-light industry sequence, but conventional stopper boiling point is higher, is dissolved in target product, cause the inhibitor concentration in de-light industry sequence excessive, polymerization inhibition effect is undesirable.
Summary of the invention
The object of the invention is to the defect overcoming prior art, provide a kind of ethyl acrylate to reclaim productive rate and the higher ethyl acrylate waste oil recovery process of finished product purity.
For achieving the above object, technical scheme of the present invention is a kind of ethyl acrylate waste oil recovery process, it is characterized in that, comprises the following steps:
S1: depolymerization, intensification depolymerization is carried out to the mixed solution of ethyl acrylate waste oil, vinylformic acid waste oil, esterified acid catalyst and isooctyl alcohol, reaction terminates to distill gained reaction solution afterwards, main component be the mixed vapour of ethyl acrylate, isooctyl alcohol and water through condensation, stratification, obtain oil phase depolymerization mixed solution;
S2: depolymerization material esterification, oil phase depolymerization mixed solution, isooctyl alcohol, vinylformic acid, toluene, esterified acid catalyst carry out esterification at esterification temperature, esterification gained esterification liquid is distilled, main component is that toluene, water and vinylformic acid steam are through condensation, stratification, gained oil phase material backflow also rectifying, separation of methylbenzene, distillation remains as esterification mixed solution;
S3: Hui Zheng, heat up to esterification mixed solution and the thick steaming of insulation under negative pressure, main component is that the steam of ethyl acrylate and isooctyl alcohol must return steaming mixed solution through condensation;
S4: neutralization, adopt liquid caustic soda to neutralize back and steam mixed solution, layering obtains in oil phase and mixed solution;
S5: de-light, to going alcohol esterifying liquid intensification underpressure distillation, vapour condensation obtains the light constituent and de-light esterifying liquid that main component is isooctyl alcohol and water;
S6: de-heavy, to de-light esterifying liquid intensification underpressure distillation, main component be ethyl acrylate distillate steam through condensation, obtain ethyl acrylate finished product.
In order to realize being separated of esterification products and higher impurity and stopper, preferred technical scheme is, the processing condition of steaming for described time are 135 ~ 145 DEG C, negative pressure-0.1 ~-0.095MPa.
Preferred technical scheme is, the processing condition of described depolymerization are 135 ~ 145 DEG C, negative pressure-0.095 ~-0.085MPa; The processing condition of described depolymerization material esterification are 125 ~ 135 DEG C, negative pressure-0.095 ~-0.085MPa; Described de-light processing condition are 110 ~ 125 DEG C, negative pressure-0.1 ~-0. 095MPa; Described de-heavy processing condition are 125 ~ 130 DEG C, negative pressure-0.1 ~-0. 095MPa.
Polymerization is very easily there is during condensation in acrylic acid and propynoic acid ester gas phase on condensing tower or pipeline, material polymerism is there is in condenser and the reactor that communicates with condenser, preferred technical scheme is, the condenser top in depolymerization material esterification step adds the esterification inhibitor solution that esterification mixed solution and stopper mix; Condenser top in described time steaming process add back steam that mixed solution and stopper mix time steam inhibitor solution; Condenser top in described de-light industry sequence adds the de-light inhibitor solution that de-light esterifying liquid and stopper mix; Condenser top in described de-heavy industry sequence adds the de-heavy inhibitor solution that ethyl acrylate finished product and stopper mix.
Preferred technical scheme is, stopper in described depolymerization inhibitor solution, esterification inhibitor solution, time steaming inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution is for being selected from least one in thiodiphenylamine, N, N-copper dibutyldithiocarbamate, Resorcinol, MEHQ.
Thiodiphenylamine generates stable thiodiphenylamine free radical by the acrylic acid and propynoic acid ester free radical of attack electron deficiency, in order to optimize the polymerization inhibition effect of depolymerization operation, preferred technical scheme is, stopper in described depolymerization inhibitor solution is thiodiphenylamine, and in described depolymerization inhibitor solution, the weight of stopper is (1 ~ 15) with the ratio of depolymerization operation phlegma weight: 10000.
Vinylformic acid is strong compared with the polymerization activity of vinylformic acid isooctyl, copper dibutyldithiocarbamate is by the mode quenching activity chain of electron transmission, thus termination polyreaction, in order to the content making the stopper proportioning of esterification step adapt to acrylic acid and propynoic acid ester, optimize polymerization inhibition effect, preferred technical scheme is, stopper in described esterification inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in described esterification inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 35 ~ 50%, in described esterification inhibitor solution, the weight of stopper is (5 ~ 30) with the ratio of oil phase depolymerization mixed solution weight: 10000.
Return in the steam of steaming process containing a small amount of vinylformic acid, in order to optimize back the polymerization inhibition effect of steaming process, preferred technical scheme is, the stopper steamed in inhibitor solution for described time is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, the weight percent steaming N, N-copper dibutyldithiocarbamate in inhibitor solution stopper for described time is 40 ~ 60%, and the weight of steaming stopper in inhibitor solution for described time is (2 ~ 25) with returning the ratio steaming mixed solution weight: 10000.
Substantially not containing vinylformic acid in steam in de-light industry sequence, in order to optimize the polymerization inhibition effect of de-light industry sequence, preferred technical scheme is, stopper in described de-light inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in described de-light inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 55 ~ 70%, in described de-light inhibitor solution stopper weight and oil phase in and the ratio of mixed solution weight be (2 ~ 16): 10000.
N, the polymerization inhibition performance of N-copper dibutyldithiocarbamate and thiodiphenylamine is better than MEHQ, and not easily decompose, be mixed in finished product not easily separated, in order to avoid the use of stopper affects end properties, preferred technical scheme is, the stopper in described de-heavy inhibitor solution is MEHQ, and in described de-heavy inhibitor solution, the weight of stopper is (1 ~ 15) with the ratio of de-light esterifying liquid weight: 10000.
Advantage of the present invention and beneficial effect are:
Ethyl acrylate waste oil recovery process of the present invention by esterification and in and add back steaming process between operation, the stopper that separate targets product propylene acid-2-ethylhexyl adds with depolymerization and esterif iotacation step, simultaneously also separable go out the impurity of other highers, be convenient to the control that de-light industry sequence stopper add-on and proportioning are selected, ensure the polymerization inhibition effect of whole ethyl acrylate recovery process.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
The raw material of embodiment 1 ethyl acrylate waste oil recovery process is ethyl acrylate waste oil and vinylformic acid waste oil, ethyl acrylate waste oil component is the vinylformic acid of 4.72%, the ethyl acrylate of 51.6%, the different monooctyl ester of 9.44%, the water of 1.6%, the own ester of octyloxy vinylformic acid 2-of 32.64%, the composition of vinylformic acid waste oil is acrylic acid dimer 38.52%, water 5.8%, vinylformic acid 55.68%, ethyl acrylate waste oil is 6:1 with the ratio of the charging capacity of vinylformic acid waste oil, drops into excessive isooctyl alcohol and carries out depolymerization reaction.
S1: depolymerization, intensification depolymerization is carried out to the mixed solution of ethyl acrylate waste oil, vinylformic acid waste oil, esterified acid catalyst (tosic acid) and isooctyl alcohol, reaction terminates to distill gained reaction solution afterwards, main component be the mixed vapour of ethyl acrylate, isooctyl alcohol and water through condensation, stratification, obtain oil phase depolymerization mixed solution;
Reaction in depolymerization operation is: the depolymerization of a part acrylic acid dimer generates two molecule vinylformic acid; Vinylformic acid and isooctyl alcohol esterification generate ethyl acrylate; The different monooctyl ester ehter bond hydrolysis of 3-octyloxy propionic acid generates Isooctyl acrylate monomer and isooctyl alcohol, and side reaction is that the direction that esterification reversible reaction generates vinylformic acid and isooctyl alcohol to hydrolysis is carried out.
S2: depolymerization material esterification, oil phase depolymerization mixed solution, isooctyl alcohol, vinylformic acid, toluene, esterified acid catalyst carry out esterification at esterification temperature, esterification gained esterification liquid is distilled, main component is that toluene, water and vinylformic acid steam are through condensation, stratification, gained oil phase material backflow also rectifying, separation of methylbenzene, distillation remains as esterification mixed solution;
The main reaction of depolymerization material esterification is: vinylformic acid and isooctyl alcohol esterification generate ethyl acrylate; To be Isooctyl acrylate monomer (ethyl acrylate) with isooctyl alcohol react generates the different monooctyl ester of 3-octyloxy propionic acid in side reaction, and Isooctyl acrylate monomer addition obtains 2 hydroxy propanoic acid isooctyl alcohol.
S3: Hui Zheng, heat up to esterification mixed solution and the thick steaming of insulation under negative pressure, main component is that the steam of ethyl acrylate and isooctyl alcohol must return steaming mixed solution through condensation;
Return the impurity containing highers such as the stopper added in esterif iotacation step and the own esters of octyloxy vinylformic acid 2-in the raffinate steamed.
S4: neutralization, adopt liquid caustic soda to neutralize back and steam mixed solution, layering obtains in oil phase and mixed solution;
The main reaction of depolymerization material esterification is: vinylformic acid and sodium hydroxide react and generates sodium acrylate, and tosic acid and sodium hydroxide react and generates paratoluenesulfonic acid sodium salt.
S5: de-light, to going alcohol esterifying liquid intensification underpressure distillation, vapour condensation obtains the light constituent and de-light esterifying liquid that main component is isooctyl alcohol and water;
S6: de-heavy, to de-light esterifying liquid intensification underpressure distillation, main component be ethyl acrylate distillate steam through condensation, obtain ethyl acrylate finished product.
Returning the processing condition of steaming is 140 DEG C, negative pressure-0.0975MPa.
The processing condition of depolymerization are 140 DEG C, negative pressure-0.09MPa; The processing condition of depolymerization material esterification are 130 DEG C, negative pressure-0.09MPa; De-light processing condition are 110 ~ 115 DEG C, negative pressure-000975MPa; De-heavy processing condition are 125 DEG C, negative pressure-0. 0975MPa.
Condenser top in depolymerization material esterification step adds the esterification inhibitor solution that esterification mixed solution and stopper mix; The condenser top returned in steaming process add back steam that mixed solution and stopper mix time steam inhibitor solution; Condenser top in de-light industry sequence adds the de-light inhibitor solution that de-light esterifying liquid and stopper mix; Condenser top in de-heavy industry sequence adds the de-heavy inhibitor solution that ethyl acrylate finished product and stopper mix.
Stopper in depolymerization inhibitor solution is thiodiphenylamine, and in depolymerization inhibitor solution, the weight of stopper is 7:10000 with the ratio of depolymerization operation phlegma weight.
Stopper in esterification inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in esterification inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 45%, and in esterification inhibitor solution, the weight of stopper is 17:10000 with the ratio of oil phase depolymerization mixed solution weight.
Returning the stopper steamed in inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, return and steam N in inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 50%, and returning the weight of steaming stopper in inhibitor solution is 13:10000 with returning the ratio steaming mixed solution weight.
Stopper in de-light inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in de-light inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 63%, in de-light inhibitor solution stopper weight and oil phase in and the ratio of mixed solution weight be 8:10000.
Stopper in de-heavy inhibitor solution is MEHQ, and in de-heavy inhibitor solution, the weight of stopper is 7:10000 with the ratio of de-light esterifying liquid weight.
Embodiment 2
Embodiment 2 is with the difference of embodiment 1: returning the processing condition of steaming is 135 DEG C, negative pressure-0.1MPa.
The processing condition of depolymerization are 135 DEG C, negative pressure-0.095MPa; The processing condition of depolymerization material esterification are 125 DEG C, negative pressure-0.095MPa; De-light processing condition are 115 ~ 120 DEG C, negative pressure-0.1MPa; De-heavy processing condition are 125 DEG C, negative pressure-0.1MPa.
Embodiment 3
Embodiment 3 is with the difference of embodiment 1: returning the processing condition of steaming is 145 DEG C, negative pressure-0.095MPa.
The processing condition of depolymerization are 145 DEG C, negative pressure-0.085MPa; The processing condition of depolymerization material esterification are 135 DEG C, negative pressure-0.085MPa; De-light processing condition are 120 ~ 125 DEG C, negative pressure-0. 095MPa; De-heavy processing condition are 130 DEG C, negative pressure-0. 095MPa.
Embodiment 4
Embodiment 4 is with the difference of embodiment 1: depolymerization inhibitor solution, esterification inhibitor solution, time stopper steamed in inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution are Resorcinol, and the consumption of stopper is identical with embodiment.
Embodiment 5
Embodiment 5 is with the difference of embodiment 4: depolymerization inhibitor solution, esterification inhibitor solution, time stopper steamed in inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution are N, N-copper dibutyldithiocarbamate, the consumption of stopper is identical with embodiment.
Embodiment 6
Embodiment 6 is with the difference of embodiment 4: depolymerization inhibitor solution, esterification inhibitor solution, time stopper steamed in inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution are thiodiphenylamine, and the consumption of stopper is identical with embodiment.
Embodiment 7
Embodiment 7 is with the difference of embodiment 4: depolymerization inhibitor solution, esterification inhibitor solution, time stopper steamed in inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution are MEHQ, and the consumption of stopper is identical with embodiment.
Embodiment 8
Embodiment 8 is with the difference of embodiment 1: the stopper in depolymerization inhibitor solution is thiodiphenylamine, and in depolymerization inhibitor solution, the weight of stopper is 1:10000 with the ratio of depolymerization operation phlegma weight.
Stopper in esterification inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in esterification inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 50%, and in esterification inhibitor solution, the weight of stopper is 30:10000 with the ratio of oil phase depolymerization mixed solution weight.
Returning the stopper steamed in inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, return and steam N in inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 60%, and returning the weight of steaming stopper in inhibitor solution is 25:10000 with returning the ratio steaming mixed solution weight.
Stopper in de-light inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in de-light inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 70%, in de-light inhibitor solution stopper weight and oil phase in and the ratio of mixed solution weight be 16:10000.
Stopper in de-heavy inhibitor solution is MEHQ, and in de-heavy inhibitor solution, the weight of stopper is 15:10000 with the ratio of de-light esterifying liquid weight.
Embodiment 9
Embodiment 9 is with the difference of embodiment 1: the stopper in depolymerization inhibitor solution is thiodiphenylamine, and in depolymerization inhibitor solution, the weight of stopper is 15:10000 with the ratio of depolymerization operation phlegma weight.
Stopper in esterification inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in esterification inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 35%, and in esterification inhibitor solution, the weight of stopper is 5:10000 with the ratio of oil phase depolymerization mixed solution weight.
Returning the stopper steamed in inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, return and steam N in inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 40%, and returning the weight of steaming stopper in inhibitor solution is 2:10000 with returning the ratio steaming mixed solution weight.
Stopper in de-light inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in de-light inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 55%, in de-light inhibitor solution stopper weight and oil phase in and the ratio of mixed solution weight be 2:10000.
Stopper in de-heavy inhibitor solution is MEHQ, and in de-heavy inhibitor solution, the weight of stopper is 1:10000 with the ratio of de-light esterifying liquid weight.
In embodiment 1-9, inhibitor solution all adopts the mode of spray to be added by condenser top, in depolymerization inhibitor solution, inhibitor concentration (weight percent concentration) is 2 ~ 2.2%, in esterification inhibitor solution, inhibitor concentration (weight percent concentration) is 1.5 ~ 1.8%, returning inhibitor concentration (weight percent concentration) in steaming inhibitor solution is 2.4 ~ 3%, in de-light inhibitor solution, inhibitor concentration (weight percent concentration) is 3 ~ 3.6%, and in de-heavy inhibitor solution, inhibitor concentration (weight percent concentration) is 0.4 ~ 0.8%.
Test-results shows, in embodiment 1-3, the ethyl acrylate productive rate of embodiment 1 is greater than embodiment 2 and embodiment 3, in embodiment 4-7, the ethyl acrylate productive rate of embodiment 5 and 6 is larger, occur white mass all in various degree, polymerization reaction take place in the condenser of embodiment 4 and 7, wherein embodiment 7 polymerization inhibition effect is the poorest.Embodiment 1,8,9 is compared, the ethyl acrylate productive rate of embodiment 1 is larger, the same polyreaction occurred in various degree in embodiment 8 and 9, N, N-copper dibutyldithiocarbamate and the thiodiphenylamine polymerization inhibition effect that makes used in combination obviously strengthen, and N, N-copper dibutyldithiocarbamate and thiodiphenylamine can be removed in de-heavy industry sequence, with employing MEHQ as compared with stopper, cost is lower.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. an ethyl acrylate waste oil recovery process, is characterized in that, comprises the following steps:
S1: depolymerization, intensification depolymerization is carried out to the mixed solution of ethyl acrylate waste oil, vinylformic acid waste oil, esterified acid catalyst and isooctyl alcohol, reaction terminates to distill gained reaction solution afterwards, main component be the mixed vapour of ethyl acrylate, isooctyl alcohol and water through condensation, stratification, obtain oil phase depolymerization mixed solution;
S2: depolymerization material esterification, oil phase depolymerization mixed solution, isooctyl alcohol, vinylformic acid, toluene, esterified acid catalyst carry out esterification at esterification temperature, esterification gained esterification liquid is distilled, main component is that toluene, water and vinylformic acid steam are through condensation, stratification, gained oil phase material backflow also rectifying, separation of methylbenzene, distillation remains as esterification mixed solution;
S3: Hui Zheng, heat up to esterification mixed solution and the thick steaming of insulation under negative pressure, main component is that the steam of ethyl acrylate and isooctyl alcohol must return steaming mixed solution through condensation;
S4: neutralization, adopt liquid caustic soda to neutralize back and steam mixed solution, layering obtains in oil phase and mixed solution;
S5: de-light, to going alcohol esterifying liquid intensification underpressure distillation, vapour condensation obtains the light constituent and de-light esterifying liquid that main component is isooctyl alcohol and water;
S6: de-heavy, to de-light esterifying liquid intensification underpressure distillation, main component be ethyl acrylate distillate steam through condensation, obtain ethyl acrylate finished product.
2. ethyl acrylate waste oil recovery process according to claim 1, is characterized in that, the processing condition of steaming for described time are 135 ~ 145 DEG C, negative pressure-0.1 ~-0.095MPa.
3. ethyl acrylate waste oil recovery process according to claim 1, is characterized in that, the processing condition of described depolymerization are 135 ~ 145 DEG C, negative pressure-0.095 ~-0.085MPa; The processing condition of described depolymerization material esterification are 125 ~ 135 DEG C, negative pressure-0.095 ~-0.085MPa; Described de-light processing condition are 110 ~ 125 DEG C, negative pressure-0.1 ~-0. 095MPa; Described de-heavy processing condition are 125 ~ 130 DEG C, negative pressure-0.1 ~-0. 095MPa.
4. ethyl acrylate waste oil recovery process according to claim 1, is characterized in that, the condenser top in depolymerization operation adds the depolymerization inhibitor solution that depolymerization phlegma and stopper mix; Condenser top in depolymerization material esterification step adds the esterification inhibitor solution that esterification mixed solution and stopper mix; Condenser top in described time steaming process add back steam that mixed solution and stopper mix time steam inhibitor solution; Condenser top in described de-light industry sequence adds the de-light inhibitor solution that de-light esterifying liquid and stopper mix; Condenser top in described de-heavy industry sequence adds the de-heavy inhibitor solution that ethyl acrylate finished product and stopper mix.
5. ethyl acrylate waste oil recovery process according to claim 4, it is characterized in that, stopper in described depolymerization inhibitor solution, esterification inhibitor solution, time steaming inhibitor solution, de-light inhibitor solution, de-heavy inhibitor solution is for being selected from least one in thiodiphenylamine, N, N-copper dibutyldithiocarbamate, Resorcinol, MEHQ.
6. ethyl acrylate waste oil recovery process according to claim 5, it is characterized in that, stopper in described depolymerization inhibitor solution is thiodiphenylamine, and in described depolymerization inhibitor solution, the weight of stopper is (1 ~ 15) with the ratio of depolymerization operation phlegma weight: 10000.
7. ethyl acrylate waste oil recovery process according to claim 5, it is characterized in that, stopper in described esterification inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in described esterification inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 35 ~ 50%, and in described esterification inhibitor solution, the weight of stopper is (5 ~ 30) with the ratio of oil phase depolymerization mixed solution weight: 10000.
8. ethyl acrylate waste oil recovery process according to claim 5, it is characterized in that, the stopper steamed in inhibitor solution for described time is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, steam N in inhibitor solution stopper described time, the weight percent of N-copper dibutyldithiocarbamate is 40 ~ 60%, and the weight of steaming stopper in inhibitor solution for described time is (2 ~ 25) with returning the ratio steaming mixed solution weight: 10000.
9. ethyl acrylate waste oil recovery process according to claim 5, it is characterized in that, stopper in described de-light inhibitor solution is N, the composition of N-copper dibutyldithiocarbamate and thiodiphenylamine, N in described de-light inhibitor solution stopper, the weight percent of N-copper dibutyldithiocarbamate is 55 ~ 70%, in described de-light inhibitor solution stopper weight and oil phase in and the ratio of mixed solution weight be (2 ~ 16): 10000.
10. ethyl acrylate waste oil recovery process according to claim 5, it is characterized in that, stopper in described de-heavy inhibitor solution is MEHQ, and in described de-heavy inhibitor solution, the weight of stopper is (1 ~ 15) with the ratio of de-light esterifying liquid weight: 10000.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108484406A (en) * | 2018-04-27 | 2018-09-04 | 江苏新东风化工科技有限公司 | A kind of Isooctyl acrylate monomer waste oil recovery process |
| CN110099891A (en) * | 2016-12-21 | 2019-08-06 | 巴斯夫欧洲公司 | By distilling the method for separating pure acrylic acid 2- ethylhexyl or pure acrylic acid 2- Propylheptyl from corresponding crude acrylic acid Arrcostab |
| 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 |
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| CN101239909A (en) * | 2008-03-17 | 2008-08-13 | 上海华谊丙烯酸有限公司 | Method for preparing (methyl) acrylate and device used for the same |
| CN201313874Y (en) * | 2008-12-16 | 2009-09-23 | 沈晓东 | Waste acrylic acid and acrylic ester recovery device |
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| CN101239909A (en) * | 2008-03-17 | 2008-08-13 | 上海华谊丙烯酸有限公司 | Method for preparing (methyl) acrylate and device used for the same |
| CN201313874Y (en) * | 2008-12-16 | 2009-09-23 | 沈晓东 | Waste acrylic acid and acrylic ester recovery device |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110099891A (en) * | 2016-12-21 | 2019-08-06 | 巴斯夫欧洲公司 | By distilling the method for separating pure acrylic acid 2- ethylhexyl or pure acrylic acid 2- Propylheptyl from corresponding crude acrylic acid Arrcostab |
| CN110099891B (en) * | 2016-12-21 | 2022-06-10 | 巴斯夫欧洲公司 | Method for separating pure 2-ethylhexyl acrylate or pure 2-propylheptyl acrylate from corresponding crude alkyl acrylate by distillation |
| CN108484406A (en) * | 2018-04-27 | 2018-09-04 | 江苏新东风化工科技有限公司 | A kind of Isooctyl acrylate monomer waste oil recovery process |
| 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 |
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| CN104892416B (en) | 2017-06-13 |
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