CN110128267A - A kind of Isooctyl acrylate monomer esterifying liquid method for washing - Google Patents
A kind of Isooctyl acrylate monomer esterifying liquid method for washing Download PDFInfo
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- CN110128267A CN110128267A CN201910541220.8A CN201910541220A CN110128267A CN 110128267 A CN110128267 A CN 110128267A CN 201910541220 A CN201910541220 A CN 201910541220A CN 110128267 A CN110128267 A CN 110128267A
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- Prior art keywords
- washing
- reaction
- acrylic acid
- acrylate monomer
- isooctyl acrylate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
It include that raw material is subjected to mixing esterification in the first reaction kettle the invention discloses a kind of Isooctyl acrylate monomer esterifying liquid method for washing, the vapour mixture obtained injection below the side of the second reaction kettle is reacted to be distilled, the alcohol steam phase obtained after distillation flows into the first reaction kettle and carries out vulcanization reaction, the residual solution obtained in second reaction kettle is mutually passed through in water scrubber, the acrylic acid that washing is completed is flowed out from water scrubber discharge port, the acidic species that the mouth discharge of water scrubber top discharge at this time hydrolyzes are added alkali and are neutralized, obtained aqueous phase is sent to progress propenyl recycling in destilling tower C1, obtain finished product acrylic acid.Esterification washing is carried out using above-mentioned steps, circular response processing is mutually carried out with waste residue to the liquid and gas generated in each step, guarantee making full use of for reactant, acrylic acid is prepared using multiple reciprocation cycle reaction simultaneously, the esterification completeness of acrylic acid is greatly improved compared to the technique being currently known.
Description
Technical field
Compact, esterification that the present invention relates to a kind of Isooctyl acrylate monomer esterifying liquid method for washing more particularly to a kind of process is instead
Answer complete Isooctyl acrylate monomer esterifying liquid method for washing.
Background technique
In previous Isooctyl acrylate monomer production process, neutralization reaction is carried out after esterification, is directly washed after not being esterified
Technique, product quality low consumption is big, is not able to satisfy production needs.Previous water scrubber is exactly to clean molten in feedstock transportation to tower body
Liquid, which is transported in tower body, carries out cleaning reaction etc. to raw material, under such water washing effect is bad, and time-consuming working efficiency, it is therefore contemplated that
Acroleic acid esterification technique improved.
Chinese patent 201610641005.1 discloses a kind of Isooctyl acrylate monomer esterifying liquid washing process, the technique be
In the presence of at least one acrylic acid stabilizer, with propenyl direct esterification acrylic acid, the esterification sulfuric acid catalysis,
Obtained crude reaction mixture B1 contains the different monooctyl ester of Isooctyl acrylate monomer, propenyl, acrylic acid, bisulphate, micro sulfuric acid
With general impurity.This technique finds esterification in process of production there is esterifications not exclusively, and waste residue rate is high asks
Topic, therefore how to improve the completeness of esterification and control the problem of waste residue rate is present invention research.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of Isooctyl acrylate monomer esterifying liquid method for washing, have process
Feature compact, esterification is complete.
In order to solve the above technical problems, the technical solution of the present invention is as follows: a kind of Isooctyl acrylate monomer esterifying liquid method for washing,
Its innovative point is that the Isooctyl acrylate monomer esterifying liquid method for washing includes the following steps:
Step is 1.: by Isooctyl acrylate monomer, propenyl, acrylic acid, the different monooctyl ester of bisulphate and sulfuric acid in the first reaction kettle
In carry out mixing esterification, reaction temperature is 80~100 DEG C, reaction time 40min, and after reaction, obtaining includes third
The vapour mixture of olefin(e) acid, propylene alcohol and water；
Step is 2.: by vapour mixture that above-mentioned steps obtain, injection is distilled below the side of the second reaction kettle,
For vapo(u)rizing temperature at 80 DEG C, distillation time 30min, the alcohol steam phase obtained after distillation, which flows into the first reaction kettle, carries out sulphur
Change reaction, the product revolving in the second reaction kettle is removed into alcohol, residue is extracted with Isooctyl acrylate monomer, then acrylic acid is different pungent
Ester is washed, and acrylic acid is obtained；
Step is 3.: the residual solution obtained in the second reaction kettle of above-mentioned steps is mutually passed through in water scrubber, is controlled by washing time
In 10min or more, the acrylic acid that washing is completed is flowed out from water scrubber discharge port, the mouth discharge of water scrubber top discharge at this time hydrolyzes
To acidic species alkali be added neutralized, obtained aqueous phase is sent in destilling tower C1 progress propenyl recycling, propenyl
Alcohol is separated from aqueous phase, obtains finished product acrylic acid.
Preferably, the different monooctyl ester of the Isooctyl acrylate monomer, propenyl, acrylic acid, bisulphate and sulfuric acid are in the first reaction
Before reacting in kettle, acrylic acid and propenyl account for 80% of reaction raw materials or more.
Preferably, the sulfuric acid is the concentrated sulfuric acid, and the concentrated sulfuric acid is the sulfuric acid solution that mass fraction is not less than 70%.
Preferably, the water lotion that washing step is carried out in the water scrubber is the mixed liquor of water and organic solvent, water and is had
Solvent accounting is 10:1, and wherein organic solvent is the secondary one or more of methanol, ethyl alcohol, ether, toluene.
Preferably, the step 3. in last phase is generated in the second reaction kettle reaction process, the last phase is that reaction is useless
Slag includes the intermediate waste residue and impurity generated in the reaction waste residue, and the reaction waste residue is mutually through the second reaction kettle side outlet
It is discharged into waste residue recyclable device.
Preferably, separating screen device is provided in the waste residue recyclable device, separating screen device cuts the impurity in reaction waste residue
It stays, the reaction waste residue passed through from separating screen device falls back to the bottom of waste residue recyclable device, then returns by discharge of pipes to solid waste
Processing center is received, the impurity after separating screen device retains is discharged into impurity recovery processing center through impurity collection conduit.
The present invention has the advantages that esterification washing is carried out using above-mentioned steps, it is gentle to the liquid phase generated in each step
Circular response processing is mutually mutually carried out with waste residue, guarantees making full use of for reactant, while reacting system using multiple reciprocation cycle
Standby to obtain acrylic acid, the esterification completeness of acrylic acid is greatly improved compared to the technique being currently known.
Specific embodiment
1. Isooctyl acrylate monomer esterifying liquid method for washing of the invention includes the following steps: step: by Isooctyl acrylate monomer,
The different monooctyl ester of propenyl, acrylic acid, bisulphate and sulfuric acid carry out mixing esterification, reaction temperature 80 in the first reaction kettle
~100 DEG C, reaction time 40min, after reaction, obtain the vapour mixture comprising acrylic acid, propylene alcohol and water；Step
2.: the vapour mixture that above-mentioned steps obtain is injected below the side of the second reaction kettle and is distilled, vapo(u)rizing temperature is 80
DEG C, distillation time 30min, the alcohol steam phase that obtains after distillation flows into the first reaction kettle and carries out vulcanization reaction, by the
Product revolving in two reaction kettles removes alcohol, and residue is extracted with Isooctyl acrylate monomer, then Isooctyl acrylate monomer is washed,
Obtain acrylic acid；Step is 3.: the residual solution obtained in the second reaction kettle of above-mentioned steps is mutually passed through in water scrubber, is controlled by washing time
In 10min or more, the acrylic acid that washing is completed is flowed out from water scrubber discharge port, the mouth discharge of water scrubber top discharge at this time hydrolyzes
To acidic species alkali be added neutralized, obtained aqueous phase is sent in destilling tower C1 progress propenyl recycling, propenyl
Alcohol is separated from aqueous phase, obtains finished product acrylic acid.Esterification washing is carried out using above-mentioned steps, to generating in each step
Liquid and gas mutually carry out circular response processing with waste residue, guarantee making full use of for reactant, while using multiple reciprocal
Circular response prepares acrylic acid, and the esterification completeness of acrylic acid is greatly improved compared to the technique being currently known.
Above-mentioned Isooctyl acrylate monomer, propenyl, acrylic acid, the different monooctyl ester of bisulphate and sulfuric acid is anti-in the first reaction kettle
Before answering, acrylic acid and propenyl account for 80% of reaction raw materials or more.Sulfuric acid is the concentrated sulfuric acid, and the concentrated sulfuric acid is not less than for mass fraction
70% sulfuric acid solution.
The water lotion that washing step is carried out in above-mentioned water scrubber is the mixed liquor of water and organic solvent, and water and organic solvent account for
Than for 10:1, wherein organic solvent is the secondary one or more of methanol, ethyl alcohol, ether, toluene.Step 3. in the second reaction kettle
Generate last phase in reaction process, the last phase is reaction waste residue, include in the reaction waste residue intermediate waste residue generated and
Impurity, the reaction waste residue are mutually discharged into waste residue recyclable device through the second reaction kettle side outlet.In waste residue recyclable device
It is provided with separating screen device, separating screen device retains the impurity in reaction waste residue, and the reaction waste residue passed through from separating screen device is fallen back to
Then the bottom of waste residue recyclable device is recycled center by discharge of pipes to solid waste, the impurity after separating screen device retains
Impurity recovery processing center is discharged into through impurity collection conduit.
Finally, it should be noted that property technical side the above examples are only used to illustrate the technical scheme of the present invention and are not limiting
Case, those skilled in the art should understand that, modification or equivalent replacement of the technical solution of the present invention are made for those, and
The objective and range for not departing from the technical program, are intended to be within the scope of the claims of the invention.
Claims (6)
1. a kind of Isooctyl acrylate monomer esterifying liquid method for washing, which is characterized in that Isooctyl acrylate monomer esterifying liquid washing side
Method includes the following steps:
Step is 1.: by Isooctyl acrylate monomer, propenyl, acrylic acid, the different monooctyl ester of bisulphate and sulfuric acid in the first reaction kettle into
Row mixing esterification, reaction temperature be 80~100 DEG C, reaction time 40min, after reaction, obtain comprising acrylic acid,
The vapour mixture of propylene alcohol and water；
Step is 2.: by vapour mixture that above-mentioned steps obtain, injection is distilled below the side of the second reaction kettle, is distilled
At 80 DEG C, distillation time 30min, the alcohol steam phase obtained after distillation flows into the first reaction kettle vulcanize anti-temperature
Answer, the product revolving in the second reaction kettle removed into alcohol, residue extracts with Isooctyl acrylate monomer, then by Isooctyl acrylate monomer into
Row washing, obtains acrylic acid；
Step is 3.: the residual solution obtained in the second reaction kettle of above-mentioned steps is mutually passed through in water scrubber, is existed by washing time control
10min or more flows out the acrylic acid that washing is completed from water scrubber discharge port, and the mouth discharge of water scrubber top discharge at this time hydrolyzes to obtain
Acidic species alkali be added neutralized, obtained aqueous phase is sent in destilling tower C1 progress propenyl recycling, propenyl alcohol
It is separated from aqueous phase, obtains finished product acrylic acid.
2. a kind of Isooctyl acrylate monomer esterifying liquid method for washing as described in claim 1, which is characterized in that the acrylic acid is different
Before the different monooctyl ester of monooctyl ester, propenyl, acrylic acid, bisulphate and sulfuric acid react in the first reaction kettle, acrylic acid and propenyl
Account for 80% or more of reaction raw materials.
3. a kind of Isooctyl acrylate monomer esterifying liquid method for washing as described in claim 1, which is characterized in that the sulfuric acid is dense
Sulfuric acid, the concentrated sulfuric acid are the sulfuric acid solution that mass fraction is not less than 70%.
4. a kind of Isooctyl acrylate monomer esterifying liquid method for washing as described in claim 1, which is characterized in that in the water scrubber
The water lotion for carrying out washing step is the mixed liquor of water and organic solvent, and water and organic solvent accounting are 10:1, wherein organic molten
Agent is one or more of methanol, ethyl alcohol, ether, toluene.
5. a kind of Isooctyl acrylate monomer esterifying liquid method for washing as described in claim 1, which is characterized in that the step 3. in
Last phase is generated in second reaction kettle reaction process, it includes in generating in the reaction waste residue that the last phase, which is reaction waste residue,
Mesosome waste residue and impurity, the reaction waste residue are mutually discharged into waste residue recyclable device through the second reaction kettle side outlet.
6. a kind of Isooctyl acrylate monomer esterifying liquid method for washing as claimed in claim 5, which is characterized in that the waste residue recycling
Separating screen device is provided in device, separating screen device retains the impurity in reaction waste residue, the reaction waste residue passed through from separating screen device
The bottom of waste residue recyclable device is fallen back to, then center is recycled by discharge of pipes to solid waste, after separating screen device retains
Impurity through impurity collection conduit be discharged into impurity recovery processing center.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910541220.8A CN110128267A (en) | 2019-06-21 | 2019-06-21 | A kind of Isooctyl acrylate monomer esterifying liquid method for washing |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910541220.8A CN110128267A (en) | 2019-06-21 | 2019-06-21 | A kind of Isooctyl acrylate monomer esterifying liquid method for washing |
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| Publication Number | Publication Date |
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| CN110128267A true CN110128267A (en) | 2019-08-16 |
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| CN201910541220.8A Withdrawn CN110128267A (en) | 2019-06-21 | 2019-06-21 | A kind of Isooctyl acrylate monomer esterifying liquid method for washing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717837A (en) * | 2021-03-23 | 2021-04-30 | 江苏国胶新材料有限公司 | High-purity isooctyl ester apparatus for producing with stirring structure |
-
2019
- 2019-06-21 CN CN201910541220.8A patent/CN110128267A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717837A (en) * | 2021-03-23 | 2021-04-30 | 江苏国胶新材料有限公司 | High-purity isooctyl ester apparatus for producing with stirring structure |
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