CN109053449A - It is a kind of that the production technology and equipments for preparing 4- hy-droxybutyl are separated by extraction - Google Patents
It is a kind of that the production technology and equipments for preparing 4- hy-droxybutyl are separated by extraction Download PDFInfo
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- CN109053449A CN109053449A CN201810672269.2A CN201810672269A CN109053449A CN 109053449 A CN109053449 A CN 109053449A CN 201810672269 A CN201810672269 A CN 201810672269A CN 109053449 A CN109053449 A CN 109053449A
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- droxybutyl
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- extraction
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- butanediol
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- 238000000605 extraction Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 42
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 7
- -1 hydroxy butyl Chemical group 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 239000003112 inhibitor Substances 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N 1,4-Benzenediol Natural products OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 5
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 3
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 14
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000000284 extract Substances 0.000 description 5
- 239000003973 paint Substances 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000007701 flash-distillation Methods 0.000 description 2
- 239000002075 main ingredient Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229940047670 sodium acrylate Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical class COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000031068 symbiosis, encompassing mutualism through parasitism Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- 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
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of are separated by extraction to prepare the production technology and equipments of 4- hy-droxybutyl, by 1,4- butanediol and acrylic acid react in the presence of catalyst, polymerization inhibitor and solvent, and primary product is 4- hy-droxybutyl and 1,4-butanediol diacrylate；It selects hexamethylene first to extract 1,4-butanediol diacrylate from water phase, then methylene chloride is selected to extract 4- acryllic acid hydroxy butyl ester, most afterwards through being evaporated under reduced pressure, finished product from water phase.The beneficial effects of the present invention are: the features such as by physical property, the content for reacting workshop section and each component of centrifugal station, devise a set of process flow, and obtain final product 4- hy-droxybutyl, purity accords demand of industrial production by the process flow.Simple process of the invention, required low energy consumption, and production cost is low, the high income of product purity height obtained and product, high-quality.
Description
Technical field
The invention belongs to field of fine chemical, especially a kind of that the production for preparing 4- hy-droxybutyl is separated by extraction
Processes and apparatus
Background technique
4- hy-droxybutyl improve resin chemical-resistant, weatherability and crosslink density, improve wetability and its
There is biggish advantage with the adhesion of polar surfaces, can be used for building coating, car paint and binder.By 4- acrylic acid hydroxyl
After the HAR and isocyanates composition acroleic acid polyurethane coating of butyl ester synthesis, the curing rate of coating is significantly improved, and paint
The properties of film, such as adhesive force, gloss, marresistance, weatherability, heat resistance, chemical-resistant, water resistance and flexibility
Deng all very excellent, 4- hy-droxybutyl has preferable application prospect in low-temperature quick-dry car refinishing paint.
Main reaction equation in 4- hy-droxybutyl synthesis technology:
Main reaction:
HO(CH2)4OH+H2C=CHCOOCH → H2C=CHCOOH (CH2)4OH+H2O
Side reaction:
HO(CH2)4OH+CH2CHCOOH→CH2CHCOO(CH2)4CH2+2H2O
In the presence of patent publication No. 101462955 discloses the catalyst such as the concentrated sulfuric acid, p-methyl benzenesulfonic acid, 1,4-butanediol with
The method that acrylic acid direct esterification prepares 1,4-butanediol diacrylate, is not described the preparation of 4- hy-droxybutyl
Method.
In the preparation of 4- hy-droxybutyl, two propylene of principal product 4- hy-droxybutyl and by-product Isosorbide-5-Nitrae butanediol
The boiling point of acid esters is close, and boiling point is not high, volatile, easily occurs containing unsaturated vinyl, when temperature is higher poly-
It closes, this just brings difficulty to isolating and purifying for product.Higher vacuum degree, temperature are needed with the method being directly evaporated under reduced pressure
The higher color that can make product is deepened, and yield reduces, and energy consumption is higher, increases cost, implements more difficult.
Summary of the invention
Overcome the deficiencies in the prior art of the present invention prepares the simple process of 4- hy-droxybutyl, and required raw material is simple,
At low cost, low energy consumption, and the high income of product purity height obtained and product, activity and flexibility are preferable, coloration, acidity, viscosity
It is low, it is high-quality.
The present invention is achieved through the following technical solutions:
It is a kind of that the production technology for preparing 4- hy-droxybutyl is separated by extraction, 1,4-butanediol and acrylic acid are being urged
It is reacted in the presence of agent, polymerization inhibitor and solvent, primary product is 4- hy-droxybutyl and 1,4-butanediol diacrylate；
It selects hexamethylene first to extract 1,4-butanediol diacrylate from water phase, then methylene chloride is selected to extract 4- third from water phase
Aenoic acid hydroxy butyl ester, most afterwards through being evaporated under reduced pressure, finished product.
The catalyst of selection is p-methyl benzenesulfonic acid, and polymerization inhibitor is hydroquinone and p-hydroxyanisole.
After extraction, 4- hy-droxybutyl is purified using rectification under vacuum mode, strict control column bottom temperature
120-150℃。
Extractant hexamethylene is recycled.
A kind of production equipment of 4- hy-droxybutyl, including sequentially connected first reactor, second reactor, first
Separator, the second separator, the first flash vessel and vacuum rectification tower；1,4- butanediol entrance and propylene is arranged in first reactor
Sour entrance, outlet are connected to second reactor, and second reactor also sets up sodium hydroxide entrance, second reactor outlet connection
First separator inlet, the first separator also set up the entrance of water, and the first separator outlet connects the second flash vessel entrance, the
Two flash vessel tower tops are connected to the first separator inlet, and another outlet of the first separator connects the second separator inlet, and second point
From the entrance that device also sets up water and extractant, the second separator one outlet output water phase, another outlet output ester is mutually dodged to first
In steaming device, the first flash vessel overhead extraction methylene chloride and water, tower bottom are connected to vacuum rectification tower, and vacuum rectification tower tower bottom produces
Object is 4- hy-droxybutyl product.
As shown in Figure 1, logistics 1 and logistics 2 are respectively reaction raw materials 1,4-butanediol and acrylic acid, the catalysis through catalyst
Effect generates 4- hy-droxybutyl and 1,4-butanediol diacrylate.
After reaction terminates, logistics 3 is rich in 4- hy-droxybutyl, 1,4-butanediol diacrylate, 1,4-butanediol
And a small amount of acrylic acid, NaOH is supplemented in by logistics 4, a small amount of acid in neutralization reaction reduces damage of the acid to equipment.
Logistics 5 after neutralizing enters Phase separation device T101 and extracts Isosorbide-5-Nitrae butanediol diacrylate, in order to make Isosorbide-5-Nitrae-
Butanediol diacrylate is preferably dissolved in extractant, and water is supplemented into T101 by logistics 6.
Logistics 7 is extraction phase, and main ingredient is extractant and 1,4-butanediol diacrylate, enters flash vessel
T105, the main component of the logistics 8 of tower top is extractant after heat exchange of flash evaporation, and extractant is preferably hexamethylene, to make to extract
Take agent that can recycle, the main component of tower base stream 9 is by-product 1,4-butanediol diacrylate.
The logistics 10 for extracting Isosorbide-5-Nitrae butanediol diacrylate enters Phase separation device T102 and extracts 4- hy-droxybutyl,
Extractant is supplemented into T102 by logistics 11, extractant is preferably methylene chloride.In order to preferably extract 4- acrylic acid hydroxyl
Butyl ester supplements water into T102 by logistics 12.Logistics 13 is water phase, and logistics 14 is ester phase, and main component is 4- acrylic acid hydroxyl
Butyl ester, there are also a small amount of not to extract complete two acrylic ester of 1,4-butanediol and undissolved Isosorbide-5-Nitrae-fourth in water phase before
Glycol.
Since extractant methylene chloride and the boiling point of the other components extracted difference are larger, logistics 14 first passes through flash vessel
T103, removes the lower component of boiling point by way of flash distillation, and the main component of overhead stream 15 is methylene chloride and water.
Tower reactor logistics 16 enter vacuum rectification tower T104, the product extracted is refined, overhead stream 17 it is main
Ingredient is 1,4-butanediol and a small amount of 1,4-butanediol diacrylate, obtains the product stream 18 for meeting technique requirement.
It is of the invention the beneficial effects of the present invention are: by physical property to reaction workshop section and each component of centrifugal station,
The features such as content, devises a set of process flow, and obtains final product 4- hy-droxybutyl by the process flow, pure
Degree complies fully with demand of industrial production.Separation of this technique for product considers the mode of rectification under vacuum after first extracting.It is reaching
Under the premise of separation requirement, separation equipment is optimized, it is determined that suitable operating parameter reduces equipment investment
And energy consumption.Simple process of the invention, required low energy consumption, and production cost is low, and product purity obtained is high and product
High income, it is high-quality.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of production equipment of the present invention.
Specific embodiment
Below by specific embodiment, the present invention is further described:
The process flow key step for the direct esterification production 4- hy-droxybutyl that the present invention designs is as follows:
React workshop section: the 1,4-butanediol for being 24.75kg/h by mass flowrate, mass flowrate are 0.3kg/h to toluene
Sulfonic acid, mass flowrate are the acrylic acid of 13.15kg/h, and mass flowrate is the hydroquinone of 0.05kg/h, and mass flowrate is
0.05kg/h this methyl ether of hydroxyl is added in reactor is reacted, and reaction product contains 52.5% 4- acrylic acid hydroxyl fourth
Ester, 10.8% Isosorbide-5-Nitrae-butanediol diacrylate, 0.19% acrylic acid, 0.01% hydroquinone and p-hydroxyanisole,
0.5% p-methyl benzenesulfonic acid, 27.6% 1,4- butanediol, 8.5% water.
After reaction terminates, logistics 3 is rich in 4- hy-droxybutyl, 1,4-butanediol diacrylate, 1,4-butanediol
And a small amount of acrylic acid, p-methyl benzenesulfonic acid, it is neutralized by logistics 4 10% NaOH, the mass flowrate of NaOH is
1.387kg/h, symbiosis is at the sodium acrylate and paratoluenesulfonic acid sodium salt of mass flowrate 0.382kg/h, and there are also unreacted quality streams
Rate is 2.689*10-5The NaOH of kg/h, so as to reduce corrosion of the acid to equipment.
Logistics 5 after neutralizing enters Phase separation device T101 and extracts 1,4-butanediol diacrylate, hexamethylene
Mass flowrate is 29.6kg/h, in order to be dissolved in 1,4-butanediol diacrylate preferably in extractant, passes through logistics 6
Water is supplemented into T101, the mass flowrate of water is 4..536kg/h, and extraction temperature is 20 DEG C.
4- hy-droxybutyl, 1,4 butanediol diacrylate, 1,4- butanediol, water, hexamethylene, hydrogen-oxygen in logistics 7
Change sodium, the mass flowrate of sodium acrylate and paratoluenesulfonic acid sodium salt is respectively 19.481kg/h, 2.244kg/h, 10.467kg/h,
29.536kg/h 0.005kg/h, 2.687*10-5Kg/hkg/h, 0.304kg/h, by returning hexamethylene after flashing, exchanging heat
It receives, flash temperature is 30 DEG C, and pressure 7kpa, extractant hexamethylene is recycled.
Entered in T102 from the logistics 10 isolated in T101, extract 4- hy-droxybutyl, by logistics 11 to
Extractant is supplemented in T102, extractant is preferably methylene chloride, and the flow of methylene chloride is 12kg/h, in order to preferably mention
4- hy-droxybutyl is taken, water is supplemented into T102 by logistics 12, the flow of water is 8kg/h.Logistics 13 is water phase, logistics
14 be ester phase, total mass flowrate 44.531kg/h, the 4- hy-droxybutyl of logistics 14,1,4-butanediol diacrylate, 1,
4- butanediol, water, methylene chloride account for 52.5%, 5%, 6.4%, 9.6%, 26.0% respectively.
Since extractant methylene chloride and the boiling point of the other components extracted difference are larger, logistics 15 first passes through flash vessel
T103, removes the lower component of boiling point by way of flash distillation, and the main component of tower top is methylene chloride and water, flash vessel
Operation temperature is 60 DEG C, pressure 1kpa.The total mass flowrate of tower reactor logistics 16 be 28.093kg/h, 4- hy-droxybutyl,
1,4 butanediol diacrylate, 1,4- butanediol, water, methylene chloride account for 77.1% respectively, 7.4%, 4.7%, 0.2%,
0.2%.
Logistics 16 enters rectifying column T104 and is refined, number of plates 10-20, preferably 14, reflux ratio 0.2-
0.5, preferably 0.35, operating pressure 0.4kpa, strict control bottom temperature, bottom temperature are 125 DEG C, and tower bottom obtains pure
The 4- hy-droxybutyl of degree 99.7%, meets demand of industrial production.
Claims (5)
1. a kind of be separated by extraction the production technology for preparing 4- hy-droxybutyl, it is characterised in that: by 1,4-butanediol and
Acrylic acid reacts in the presence of catalyst, polymerization inhibitor, and primary product is 4- hy-droxybutyl and 1,4-butanediol diacrylate
Ester；It selects hexamethylene first to extract 1,4-butanediol diacrylate from water phase, then methylene chloride is selected to extract 4- from water phase
Acryllic acid hydroxy butyl ester, most afterwards through being evaporated under reduced pressure, finished product.
2. a kind of as claimed in claim 1 be separated by extraction the production technology for preparing 4- hy-droxybutyl, feature
Be: the catalyst of selection is p-methyl benzenesulfonic acid, and polymerization inhibitor is hydroquinone and p-hydroxyanisole.
3. a kind of as claimed in claim 1 be separated by extraction the production technology for preparing 4- hy-droxybutyl, feature
It is: after extraction, 4- hy-droxybutyl is purified using rectification under vacuum mode, strict control column bottom temperature 120-
150℃。
4. a kind of as claimed in claim 1 be separated by extraction the production technology for preparing 4- hy-droxybutyl, feature exists
In: extractant hexamethylene is recycled.
5. a kind of production equipment of 4- hy-droxybutyl, it is characterised in that: instead including sequentially connected first reactor, second
Answer device, the first separator, the second separator, the first flash vessel and vacuum rectification tower；First reactor setting 1,4-butanediol enters
Mouth and acrylic acid entrance, outlet are connected to second reactor, and second reactor also sets up sodium hydroxide entrance, and second reactor goes out
Mouth the first separator inlet of connection, the first separator also set up the entrance of water, and the first separator outlet connects the second flash vessel and enters
Mouthful, the second flash vessel tower top is connected to the first separator inlet, and another outlet of the first separator connects the second separator inlet, the
Two separators also set up the entrance of water and extractant, the second separator one outlet output water phase, and another outlet exports ester mutually to the
In one flash vessel, the first flash vessel overhead extraction methylene chloride and water, tower bottom are connected to vacuum rectification tower, vacuum rectification tower tower bottom
Product is 4- hy-droxybutyl product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810672269.2A CN109053449A (en) | 2018-06-26 | 2018-06-26 | It is a kind of that the production technology and equipments for preparing 4- hy-droxybutyl are separated by extraction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810672269.2A CN109053449A (en) | 2018-06-26 | 2018-06-26 | It is a kind of that the production technology and equipments for preparing 4- hy-droxybutyl are separated by extraction |
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| Publication Number | Publication Date |
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| CN109053449A true CN109053449A (en) | 2018-12-21 |
Family
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| CN201810672269.2A Pending CN109053449A (en) | 2018-06-26 | 2018-06-26 | It is a kind of that the production technology and equipments for preparing 4- hy-droxybutyl are separated by extraction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872231A (en) * | 2019-12-09 | 2020-03-10 | 万华化学集团股份有限公司 | Preparation and separation method of 6-hydroxyhexyl acrylate |
| CN111302934A (en) * | 2020-03-19 | 2020-06-19 | 万华化学集团股份有限公司 | Preparation and separation method of 6-hydroxyhexyl acrylate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07126214A (en) * | 1993-10-29 | 1995-05-16 | Mitsubishi Chem Corp | Production of 4-hydroxybutyl acrylate |
| JP2007254384A (en) * | 2006-03-23 | 2007-10-04 | Nippon Shokubai Co Ltd | Method for producing hydroxyalkyl (meth)acrylate |
-
2018
- 2018-06-26 CN CN201810672269.2A patent/CN109053449A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07126214A (en) * | 1993-10-29 | 1995-05-16 | Mitsubishi Chem Corp | Production of 4-hydroxybutyl acrylate |
| JP2007254384A (en) * | 2006-03-23 | 2007-10-04 | Nippon Shokubai Co Ltd | Method for producing hydroxyalkyl (meth)acrylate |
Non-Patent Citations (2)
| Title |
|---|
| 化工百科全书编辑委员会: "《化工百科全书 第19卷》", 30 September 1998, 化学工业出版社 * |
| 钱逢麟 等: "《涂料助剂 品种和性能手册》", 30 November 1990, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110872231A (en) * | 2019-12-09 | 2020-03-10 | 万华化学集团股份有限公司 | Preparation and separation method of 6-hydroxyhexyl acrylate |
| CN110872231B (en) * | 2019-12-09 | 2022-02-18 | 万华化学集团股份有限公司 | Preparation and separation method of 6-hydroxyhexyl acrylate |
| CN111302934A (en) * | 2020-03-19 | 2020-06-19 | 万华化学集团股份有限公司 | Preparation and separation method of 6-hydroxyhexyl acrylate |
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Application publication date: 20181221 |