CN114716316A - Semi-continuous acrylic acid and ester heavy component recovery process - Google Patents
Semi-continuous acrylic acid and ester heavy component recovery process Download PDFInfo
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- CN114716316A CN114716316A CN202210287489.XA CN202210287489A CN114716316A CN 114716316 A CN114716316 A CN 114716316A CN 202210287489 A CN202210287489 A CN 202210287489A CN 114716316 A CN114716316 A CN 114716316A
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- 238000011084 recovery Methods 0.000 title claims abstract description 37
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 31
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 150000002148 esters Chemical class 0.000 title claims abstract description 19
- 238000005336 cracking Methods 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011265 semifinished product Substances 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 11
- 239000003112 inhibitor Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000010025 steaming Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 18
- 239000002699 waste material Substances 0.000 claims description 15
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical group CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 8
- 229950000688 phenothiazine Drugs 0.000 claims description 8
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 125000001484 phenothiazinyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001502 supplementing effect Effects 0.000 abstract 1
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 22
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 description 7
- -1 acrylic ester Chemical class 0.000 description 7
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000009089 cytolysis Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- YLYBTZIQSIBWLI-UHFFFAOYSA-N octyl acetate Chemical group CCCCCCCCOC(C)=O YLYBTZIQSIBWLI-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a semi-continuous acrylic acid and ester heavy component recovery process, and relates to the technical field of chemical component recovery. The acrylic acid and ester heavy component recovery process mainly comprises the steps of mixing a raw material with a catalyst and a polymerization inhibitor, then placing the mixture in a cracking kettle for cracking, detecting the concentration of a cracking product in the cracking recovery process, supplementing the catalyst according to a detection result, and then carrying out back steaming on the recovered product to improve the purity, so that a good recovery effect and efficiency are achieved. The invention overcomes the defects of the prior art, adopts a semi-continuous production process, reduces energy consumption, reduces the dosage of the catalyst and improves the quality of the recovered semi-finished product.
Description
Technical Field
The invention relates to the technical field of chemical component recovery, in particular to a semi-continuous acrylic acid and ester heavy component recovery process.
Background
Acrylic acid is an important organic synthetic raw material and synthetic resin monomer, and is a vinyl monomer having a very high polymerization rate. Is the simplest unsaturated carboxylic acid, consisting of one vinyl group and one carboxyl group. Pure acrylic acid is a colorless clear liquid with a characteristic pungent odor. It is miscible with water, alcohols, ethers and chloroform and is prepared from propylene obtained from an oil refinery. Most of them are used for producing acrylic esters such as methyl acrylate, ethyl acrylate, butyl acrylate, hydroxyethyl acrylate, etc. Acrylic acid and acrylic ester can be homopolymerized and copolymerized, and the polymer is used in the industrial departments of synthetic resin, synthetic fiber, super absorbent resin, building material, paint and the like.
The same acrylic esters and acrylic acid have important positions in the field of materials, the capacity release of the acrylic acid and ester industry at home and abroad is rapidly increased in recent years, the competitive pressure is high, and scientific and technological work at home and abroad is dedicated to researching how to reduce the energy consumption and material consumption of the production of the acrylic esters, wherein the recovery of the acrylic acid and the heavy components of the acrylic esters is important.
The existing recovery process generally adopts a continuous recovery process, namely, heavy components and a catalyst are continuously added according to a certain flow in the production process, the temperature of a kettle is kept at about 180 ℃, and waste residues are discharged at any time. The production process needs to be heated by steam all the time, the catalyst dosage is high, the product quality is unstable, the ester content is about 40 percent, and great waste is caused.
Aiming at the waste application No. 201910316778.6, a process and a device for recovering heavy components of n-butyl acrylate are disclosed, wherein a special device is arranged to realize the recovery process of light components and residual heavy components of the n-butyl acrylate cracking, but the recovery mode is also a continuous recovery mode and only simple recovery and utilization of the n-butyl acrylate, and the stability of the n-butyl ester content in the recovered product is poor, and the application No. 201811587283.9 discloses a method for recovering the heavy components of methyl acrylate, wherein the recovered components are obtained after the raw materials are reacted with methanol and water and then cracked for multiple times, the operation process is complex, the recovery rate of the subsequent finished products is about 70 percent, and the purity of the recovered components is not determined, so that great troubles are brought to the actual application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a semi-continuous acrylic acid and ester heavy component recovery process, which adopts a semi-continuous production process, reduces energy consumption, reduces the consumption of a catalyst and improves the purity of a recovered semi-finished product.
In order to achieve the purpose, the technical scheme of the invention is realized by the following technical scheme:
a semi-continuous acrylic acid and ester heavy component recovery process, comprising the steps of:
(1) mixing raw materials: adding the raw materials into a cracking kettle, adding a catalyst and a polymerization inhibitor, and mixing;
(2) detection and adjustment: raising the temperature of the cracking kettle to the cracking temperature, controlling the discharging speed, sampling and analyzing at intervals, adding a catalyst into the reaction kettle according to an analysis result until the reaction is finished, and discharging residues to obtain a coarse material for later use;
(3) back steaming: and (3) placing the coarse material into a reaction kettle, continuously adding a polymerization inhibitor, heating and ensuring the vacuum degree in the kettle, carrying out heat preservation distillation, then sampling and analyzing, cooling after the coarse material is qualified, discharging waste residues, obtaining a semi-finished product to be purified, and completing recovery.
Preferably, the starting material is an acrylic acid or acrylate heavy component.
Preferably, the addition amount of the catalyst in the raw material mixing process is 0.8-1.2% of the total amount of the raw materials, and after the purity of the components of the sample is reduced by sampling and analyzing, the catalyst with the total amount of 0.2-0.4% of the raw materials is continuously added into the cracking kettle.
Preferably, the catalyst is a methanesulfonic acid catalyst, and the polymerization inhibitor is phenothiazine.
Preferably, the cracking temperature in the step (2) is 160-.
Preferably, in the detection adjustment step, the cracking raw material in the cracking kettle is collected in a receiving tank after passing through a packed tower and a condenser, and a sample in the receiving tank is subjected to purity analysis.
Preferably, the receiving tank starts a vacuum system when the cracking process in the reaction kettle is carried out.
Preferably, the temperature of the steam-back in the step (3) is 110-.
Preferably, the residue and the waste residue in the recovery process are discharged and then incinerated in a waste liquid incinerator.
The invention provides a semi-continuous acrylic acid and ester heavy component recovery process, which has the advantages compared with the prior art that:
(1) according to the method, the raw materials are directly mixed with a small amount of catalyst for cracking, and the catalyst is continuously added according to the detection result of the recovered materials after actual cracking, so that the actual catalytic cracking effect is effectively improved, the use cost of the catalyst is reduced, and the production cost is reduced;
(2) this application evaporates the processing with the raw materials after the schizolysis back, evaporates the lower temperature of in-process adoption relative cracking temperature back, has reduced the energy consumption, effectively promotes the follow-up purity that obtains the material simultaneously to guarantee the rate of recovery of raw materials, effective reduce cost.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a flow chart of the apparatus of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the production process of the isooctyl acrylate comprises the following steps:
(1) preparing quantitative isooctyl acrylate heavy component in a cracking kettle, adding a methanesulfonic acid catalyst accounting for 1 percent of the mass of the isooctyl acrylate heavy component and a phenothiazine polymerization inhibitor accounting for 2 percent of the mass of the isooctyl acrylate heavy component, and uniformly mixing;
(2) starting a receiving tank vacuum system, adjusting jacket heat-conducting oil to control the temperature in the cracking kettle within the temperature range of 160-190 ℃, controlling the discharging speed to ensure that the raw material is cracked and then collected in a receiving tank through a packed tower and a condenser to obtain coarse material, sampling and analyzing the coarse material every 6 hours, and when the purity in the analysis result is lower (less than 85 percent), continuously adding a methanesulfonic acid catalyst with the mass of 0.3 percent of the original isooctyl acrylate heavy component into the cracking kettle;
(3) pumping the coarse materials in the receiving tank into a reaction kettle by a pump, adding phenothiazine into the kettle, heating, starting a vacuum system to ensure the vacuum degree in the kettle, keeping the temperature of the kettle at 110-130 ℃, keeping the temperature for 3 hours, sampling and analyzing, and cooling the cracking kettle after the coarse isooctyl ester is qualified (more than 90%);
(4) and transferring the crude isooctyl ester to an isooctyl acrylate semi-finished product tank by using a pump to be purified, wherein the total amount of the semi-finished product is 78.2 percent of the total amount of the original isooctyl acrylate heavy component, and carrying out back steaming and incineration treatment on reaction residues and waste materials obtained in an early cracking kettle in a waste liquid incinerator.
Example 2:
production process of n-butyl acrylate:
(1) preparing a certain amount of n-butyl acrylate heavy component in a cracking kettle, adding a methanesulfonic acid catalyst accounting for 0.8 percent of the mass of the n-butyl acrylate heavy component and a phenothiazine polymerization inhibitor accounting for 2 percent of the mass of the n-butyl acrylate heavy component, and uniformly mixing;
(2) starting a receiving tank vacuum system, adjusting jacket heat-conducting oil to control the temperature in the cracking kettle within the temperature range of 160-;
(3) pumping the coarse materials in the receiving tank into a reaction kettle by a pump, adding phenothiazine into the kettle, heating, starting a vacuum system to ensure the vacuum degree in the kettle, keeping the temperature of the kettle at 110-130 ℃, keeping the temperature for 3 hours, sampling and analyzing, and cooling the cracking kettle after the coarse n-butyl ester is qualified (more than 90%);
(4) and transferring the crude n-butyl acrylate to an n-butyl acrylate semi-finished product tank by a pump for purification, wherein the total amount of the semi-finished product is 77.7 percent of the total amount of the original n-butyl acrylate heavy component, and carrying out back evaporation and incineration treatment on reaction residues and waste materials obtained in the early-stage cracking kettle in a waste liquid incinerator.
Example 3:
production process of methyl acrylate:
(1) preparing a certain amount of methyl acrylate heavy component in a cracking kettle, adding a methanesulfonic acid catalyst accounting for 1.2% of the mass of the methyl acrylate heavy component and a phenothiazine polymerization inhibitor accounting for 2% of the mass of the methyl acrylate heavy component, and uniformly mixing;
(2) starting a receiving tank vacuum system, adjusting jacket heat-conducting oil to control the temperature in the cracking kettle within the temperature range of 160-190 ℃, controlling the discharging speed to ensure that the raw material is cracked and then passes through a packing tower and a condenser to be collected in a receiving tank to obtain coarse material, sampling and analyzing the coarse material every 3 hours, and when the purity in the analysis result is lower (less than 85 percent), continuously adding methyl acrylate heavy component and 0.2 percent of methanesulfonic acid catalyst by mass into the cracking kettle;
(3) pumping the coarse materials in the receiving tank into a reaction kettle by a pump, adding phenothiazine into the kettle, heating, starting a vacuum system to ensure the vacuum degree in the kettle, keeping the temperature of the kettle at 110-130 ℃, keeping the temperature for 3 hours, sampling and analyzing, and cooling the cracking kettle after the coarse methyl acrylate is qualified (more than 90%);
(4) and (3) transferring the crude methyl acrylate to a methyl acrylate semi-finished product tank by using a pump to be purified, wherein the total amount of the semi-finished product is 75.4% of the total amount of the original n-butyl acrylate heavy component, and carrying out back steaming and incineration treatment on reaction residues and waste materials obtained in the early-stage cracking kettle in a waste liquid incinerator.
And (3) detection:
1. the isooctyl ester content in the semi-finished product of example 1, the n-butyl ester content in the semi-finished product of example 2, the methyl acrylate content in the semi-finished product of example 3, and the recovery rates of the respective components in the respective examples (recovery rate is the ratio of the semi-finished product to the total raw material x the content of the material component in the semi-finished product, one decimal place is retained) were measured, respectively, and the results are shown in the following table 1:
TABLE 1
The above table shows that the process of the invention can effectively improve the recovery rate of the acrylic acid and the acrylic ester heavy components, improve the purity of the recovered products and effectively reduce the production cost.
2. The data analyzed in example 1, sampled every 6 hours during the lysis phase, were recorded (four times in total) and the results are shown in table 2 below:
TABLE 2
| Group of | First time of detection | Second detection | Third time of detection | Fourth time of detection |
| Water content% | 0.21 | 0.27 | 0.20 | 0.20 |
| Octanol% | 6.3941 | 7.0313 | 5.6618 | 6.3960 |
| Octyl ester% | 89.5322 | 89.4279 | 89.0578 | 89.4811 |
| Acrylic acid% | 0.3525 | 0.5569 | 1.2879 | 0.4041 |
| The heavy component% | 2.5182 | 1.7155 | 2.8212 | 2.4937 |
| Acetic acid octyl% | 0.1322 | 0.1362 | 0.1538 | 0.1299 |
| Toluene% | 0.000 | 0.000 | 0.000 | 0.000 |
| Unknown 1% | 0.7067 | 0.7047 | 0.6967 | 0.7198 |
| Unknown 2% | 0.1546 | 0.1508 | 0.1138 | 0.1638 |
As can be seen from the above table, the concentration of octyl ester in the sample obtained before the back steaming is lower than that after the back steaming, which indicates that the back steaming step can effectively improve the purity in the product recovery process, thereby further facilitating the subsequent production and processing.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A semi-continuous acrylic acid and ester heavy component recovery process is characterized by comprising the following steps:
(1) mixing raw materials: adding the raw materials into a cracking kettle, adding a catalyst and a polymerization inhibitor, and mixing;
(2) detection and adjustment: raising the temperature of the cracking kettle to the cracking temperature, controlling the discharging speed, sampling and analyzing at intervals, adding a catalyst into the reaction kettle according to an analysis result until the reaction is finished, and discharging residues to obtain a coarse material for later use;
(3) back steaming: and (3) placing the coarse material into a reaction kettle, continuously adding a polymerization inhibitor, heating and ensuring the vacuum degree in the kettle, carrying out heat preservation distillation, then sampling and analyzing, cooling after the coarse material is qualified, discharging waste residues, obtaining a semi-finished product to be purified, and completing recovery.
2. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: the raw material is acrylic acid or acrylate heavy component.
3. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: the adding amount of the catalyst in the raw material mixing process is 0.8-1.2% of the total amount of the raw materials, and after the purity of the components of the sample is reduced by sampling and analyzing, the catalyst with the total amount of 0.2-0.4% of the raw materials is continuously added into the cracking kettle.
4. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: the catalyst is a methanesulfonic acid catalyst, and the polymerization inhibitor is phenothiazine.
5. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: the cracking temperature in the step (2) is 160-.
6. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: in the detection and adjustment step, cracking raw materials of the cracking kettle are collected in a receiving tank after passing through a packed tower and a condenser, and a sample in the receiving tank is subjected to purity analysis.
7. The semi-continuous acrylic acid and ester heavy component recovery process of claim 6, wherein: the receiving tank starts a vacuum system when the cracking process in the reaction kettle is carried out.
8. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: the temperature of the back steaming in the step (3) is 110-130 ℃, and the sampling time is after the heat preservation back steaming is carried out for 3 h.
9. The semi-continuous acrylic acid and ester heavy component recovery process of claim 1, wherein: and in the recovery process, the residues and the waste residues are discharged and then are incinerated in a waste liquid incinerator.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN207391316U (en) * | 2017-10-19 | 2018-05-22 | 山东开泰石化丙烯酸有限公司 | A kind of butyl acrylate heavy constituent cracking system |
| CN109942424A (en) * | 2019-04-19 | 2019-06-28 | 泰兴金江化学工业有限公司 | A kind of n-butyl acrylate heavy constituent recovery process and device |
| CN110372509A (en) * | 2019-07-19 | 2019-10-25 | 江门谦信化工发展有限公司 | A kind of cracking recovery process of n-butyl acrylate heavy constituent |
| CN111362786A (en) * | 2018-12-25 | 2020-07-03 | 万华化学集团股份有限公司 | Method for recycling methyl acrylate heavy component |
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2022
- 2022-03-23 CN CN202210287489.XA patent/CN114716316A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN207391316U (en) * | 2017-10-19 | 2018-05-22 | 山东开泰石化丙烯酸有限公司 | A kind of butyl acrylate heavy constituent cracking system |
| CN111362786A (en) * | 2018-12-25 | 2020-07-03 | 万华化学集团股份有限公司 | Method for recycling methyl acrylate heavy component |
| CN109942424A (en) * | 2019-04-19 | 2019-06-28 | 泰兴金江化学工业有限公司 | A kind of n-butyl acrylate heavy constituent recovery process and device |
| CN110372509A (en) * | 2019-07-19 | 2019-10-25 | 江门谦信化工发展有限公司 | A kind of cracking recovery process of n-butyl acrylate heavy constituent |
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Application publication date: 20220708 |