CN108383725A - It is a kind of（Methyl）The continuous producing apparatus of hydroxy-ethyl acrylate - Google Patents
It is a kind of（Methyl）The continuous producing apparatus of hydroxy-ethyl acrylate Download PDFInfo
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- CN108383725A CN108383725A CN201810058898.6A CN201810058898A CN108383725A CN 108383725 A CN108383725 A CN 108383725A CN 201810058898 A CN201810058898 A CN 201810058898A CN 108383725 A CN108383725 A CN 108383725A
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- methyl
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- hydroxy
- ethyl acrylate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/24—Preparation of carboxylic acid esters by reacting carboxylic acids or derivatives thereof with a carbon-to-oxygen ether bond, e.g. acetal, tetrahydrofuran
- C07C67/26—Preparation of carboxylic acid esters by reacting carboxylic acids or derivatives thereof with a carbon-to-oxygen ether bond, e.g. acetal, tetrahydrofuran with an oxirane ring
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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
- C07C67/52—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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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of continuous producing apparatus of (methyl) hydroxy-ethyl acrylate, including material-compound tank, measuring tank, tubular reactor, condenser, intermediate maturity tank, vacuum spraying absorption tower, short-path distillation kettle, finished pot and distillation still, (methyl) acrylic acid, catalyst and polymerization inhibitor enter tubular reactor via material-compound tank, and ethylene oxide enters tubular reactor via measuring tank；Reaction mixture enters the condensed separation of condenser, and excess ethylene oxide returns to measuring tank from condenser, and semi-finished product enter intermediate maturity tank, vacuum spraying absorption tower from condenser, returns to material-compound tank from tower top, short-path distillation kettle is delivered to from bottom of tower；Three tunnels of short-path distillation kettle discharge port point, the first via to finished pot, the second tunnel returns again to short-path distillation kettle；The raffinate come out again from short-path distillation kettle enters distillation still through third road.The advantage of the invention is that：Reaction temperature is low, and side reaction is reduced, and reduces the loss of raw material, improves the conversion ratio of raw material, realizes continuous production.
Description
Technical field
The present invention relates to organic compound production equipment technologies, are more particularly to a kind of (methyl) hydroxy-ethyl acrylate
Continuous producing apparatus.
Background technology
(methyl) hydroxy-ethyl acrylate is a kind of important industrial chemicals, due to different carbon chain double bond, hydroxyl and ester
The unique texture of base, can be through homopolymerization and copolymerization multiple polymers as polymerized monomer, and such polymer bonding is securely, no
It easily peels off, is flexible and flexible at room temperature, while there is good water resistance, therefore being widely used in synthesizing (methyl) propylene
Acid resin, light-cured resin, optical resin, coating etc..
Ferric rhodanate, four are mainly added in industrial production (methyl) hydroxy-ethyl acrylate in (methyl) acrylic acid at present
Ammonio methacrylate etc. and a little hydroquinone, are heated with stirring to 90 DEG C, under nitrogen protection, are passed through ethylene oxide gas precursor reactant about
Reaction product is cooled to 60 DEG C, is evaporated under reduced pressure after adding a small amount of hydroquinone by 2h, collect 86-89 DEG C of (0.67kPa) fraction up at
Product, 80% or more yield, such equipment is disadvantageous in that ethylene oxide is inflammable and explosive, requires production equipment stringent.Mesh
Before, for realizing industrial production (methyl) hydroxy-ethyl acrylate, existing device there are it is seriously polluted, cannot achieve continuous production
The problems such as.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of free of contamination (methyl) hydroxy-ethyl acrylate
Continuous producing apparatus.
The present invention is to solve above-mentioned technical problem by the following technical programs：
A kind of continuous producing apparatus of (methyl) hydroxy-ethyl acrylate, including it is material-compound tank, measuring tank, tubular reactor, cold
Condenser, intermediate maturity tank, vacuum spraying absorption tower, short-path distillation kettle, finished pot and distillation still, (methyl) acrylic acid, catalyst
Enter tubular reactor via material-compound tank with polymerization inhibitor, ethylene oxide enters tubular reactor via measuring tank, (methyl) propylene
Acid, ethylene oxide, catalyst and polymerization inhibitor certain pressure, at a temperature of ring-opening reaction is carried out in tubular reactor, be made anti-
Answer mixed liquor；Reaction mixture enters that condenser is condensed to isolate excess ethylene oxide and semi-finished product (methyl) acrylic acid hydroxyl second
Ester, excess ethylene oxide is from condenser back to measuring tank to recycle excess ethylene oxide, semi-finished product (methyl) acrylic acid
Hydroxyl ethyl ester enters intermediate maturity tank from condenser；Semi-finished product (methyl) hydroxy-ethyl acrylate enters vacuum spraying from intermediate finished pot
Absorption tower tower top, deviates from (methyl) acrylic acid under vacuum condition on column plate from tower top, and (methyl) acrylic acid of abjection returns to
Material-compound tank deviates from thick (methyl) hydroxy-ethyl acrylate finished and is delivered to progress short distance rectifying in short-path distillation kettle from bottom of tower；It is short
Three tunnels of journey distillation still discharge port point, the first via to finished pot, the second tunnel returns again to short-path distillation kettle；Go out again from short-path distillation kettle
The raffinate come enters distillation still through third road and carries out distillation reaction.Wherein, (methyl) acrylic acid is methacrylic acid or propylene
Acid, (methyl) hydroxy-ethyl acrylate refer to hydroxyethyl methacrylate or hydroxy-ethyl acrylate.
Preferably, (methyl) acrylic acid passes through canned motor pump, regulating valve, (methyl) acrylic acid mass flowmenter via material-compound tank
Into tubular reactor, canned motor pump tail pipe is connected to material-compound tank to constitute (methyl) acrylic acid cycle；Ethylene oxide is via measuring tank
Enter tubular reactor by metering pump, surge tank, ethylene oxide mass flow meter, metering pump is connected to measuring tank to constitute epoxy
Ethane recycle.
Preferably, cycle water coil is set in material-compound tank, is cooled down by material-compound tank of recirculated water, it is more than ring after 40 DEG C to prevent temperature
Oxidative ethane reacts under the action of catalyst with (methyl) acrylic acid.
Preferably, thermometer is set on tubular reactor and shell side recirculated water is chain, to control reactor cycles coolant-temperature gage,
Stablize temperature of reactor, ensures reaction safety.
Preferably, polymerization inhibitor is added into intermediate maturity tank, to prevent from reacting in intermediate maturity tank.
Preferably, intermediate maturity pot bottom sets sample tap, to chemically examine intermediate maturity ingredient, to by mass flowmenter come
Adjust ethylene oxide and (methyl) acrylic acid rate of charge.
Preferably, the extraction duct that (methyl) acrylic acid of abjection is sprayed via (methyl) acrylic acid returns to after absorbing matches
Batch can；Deviate from thick (methyl) hydroxy-ethyl acrylate finished through bottom of tower discharging pump, discharging condenser cooling, be sent into semi-finished product tank,
It is then sent to short-path distillation kettle and carries out short distance rectifying.
Preferably, finished product and a raffinate are obtained after short distance rectifying, three tunnels of short-path distillation kettle discharging point, the first via is from bottom
Discharge port is to finished pot to store finished product；Second road from kettle side discharge port through a residual liquid tank return again to short-path distillation kettle carry out it is short
Journey rectifying, a residual liquid tank is for storing a raffinate；The secondary raffinate come out again from short-path distillation kettle is from kettle side discharge port
Secondary residual liquid tank is passed sequentially through through third road, raffinate gravity tank enters distillation still, wherein secondary raffinate is beaten through pump to a raffinate high position
Tank enters distillation still by gravity tank gravity flow and carries out distillation reaction.
Preferably, after distillation reaction gained product of distillation reenter a residual liquid tank, again return to short-path distillation kettle into
Row short distance rectifying；To make short-path distillation and distillation, cycle carries out successively, high level finished product is made, realizes continuous production.
The method that (methyl) hydroxy-ethyl acrylate is produced using the continuous producing apparatus of above-mentioned (methyl) hydroxy-ethyl acrylate,
Include the following steps：(methyl) acrylic acid, catalyst and polymerization inhibitor are put into tubular reactor via material-compound tank, by ethylene oxide
Tubular reactor is put into via measuring tank, ring-opening reaction is carried out in tubular reactor, reaction mixture is made；Reaction is set to mix
Liquid enters that condenser is condensed to isolate excess ethylene oxide and semi-finished product (methyl) hydroxy-ethyl acrylate, excess ethylene oxide from
Condenser returns to measuring tank, and semi-finished product (methyl) hydroxy-ethyl acrylate enters intermediate maturity tank from condenser；To intermediate maturity
Polymerization inhibitor is added in tank, semi-finished product (methyl) hydroxy-ethyl acrylate enters vacuum spraying absorption tower from intermediate finished pot, in column plate
Deviate from (methyl) acrylic acid from tower top under upper vacuum condition, (methyl) acrylic acid of abjection returns to material-compound tank, deviates to finish
Slightly (methyl) hydroxy-ethyl acrylate is delivered to progress short distance rectifying in short-path distillation kettle from bottom of tower；The discharging of short-path distillation kettle is finished product
With a raffinate, finished product to finished pot, a raffinate returns again to the progress short distance rectifying of short-path distillation kettle after entering a residual liquid tank,
Finished product and secondary raffinate are obtained, secondary raffinate passes sequentially through secondary residual liquid tank, raffinate gravity tank enters distillation still and distill instead
It answers.
The present invention has the following advantages compared with prior art：The reaction temperature of the production equipment of the present invention is low, and side reaction subtracts
It is few, the loss of raw material is reduced, the conversion ratio of raw material is improved, so that product quality has obtained further being promoted；Institute
It throws equipment and uses whole process DCS control systems, high degree of automation, technique is advanced, and production efficiency is higher；Raw material and finished product are whole
Using tank storage, pipeline disengaging, entire production link all carries out in closed environment, without exhaust gas, waste water, by-product produce
It is raw, there is no any pollution to environment；It is especially prominent in terms of energy-saving and emission-reduction, the temperature of entire production link all 90 degrees Celsius with
Under, energy consumption substantially reduced more in the past, met the national requirement to chemical enterprise energy-saving and emission-reduction at present；And it waste water, gives up
Useful component in gas, waste residue all recycles out, empties back into system and uses.
Description of the drawings
Fig. 1 is the continuous producing apparatus figure of the application (methyl) hydroxy-ethyl acrylate.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention
Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
As shown in Figure 1, (methyl) acrylic acid is controlled certain stream by canned motor pump, regulating valve, mass flowmenter through material-compound tank
Amount enters tubular reactor, and catalyst and polymerization inhibitor enter tubular reactor through material-compound tank；Cycle water coil is set in material-compound tank, with
Circulating water cooling, prevent temperature be more than after 40 DEG C ethylene oxide react under the action of catalyst with (methyl) acrylic acid, by
Canned motor pump tail pipe back ingredient tank constitutes (methyl) acrylic acid cycle, to ensure temperature of charge in material-compound tank.
By tank field be delivered to the ethylene oxide of workshop measuring tank through metering pump, surge tank, that mass flowmenter enters tubular type is anti-
Answer device.To ensure that ethylene oxide flow, ethylene oxide separate from metering pump and return measuring tank all the way；Ethylene oxide measuring tank be it is micro- just
Nitrogen mediation valve is arranged in press operation, device top, and when pressure is less than 5Kpa, unlatching regulating valve supplements nitrogen；When pressure is higher than
5Kpa is scavenged by blow valve.
(methyl) acrylic acid, ethylene oxide, catalyst and polymerization inhibitor in tubular reactor, certain pressure, at a temperature of,
Successive reaction generates (methyl) hydroxy-ethyl acrylate.Thermometer is set on tubular reactor and shell side recirculated water is chain, and control is anti-
Device circulating water temperature is answered, temperature of reactor is stablized, ensures reaction safety.
By reactor Lai (methyl) hydroxy-ethyl acrylate mixing liquid condensed device separation excess ethylene oxide and (first
Base) hydroxy-ethyl acrylate, the ethylene oxide isolated be recycled to ethylene oxide measuring tank recycling, semi-finished product (methyl) propylene
Sour hydroxyl ethyl ester is into intermediate maturity tank.Polymerization inhibitor is added into intermediate maturity tank, to prevent from reacting in intermediate maturity tank.
Intermediate maturity pot bottom sets a sample tap, chemically examines intermediate maturity ingredient, is thrown with this to adjust ethylene oxide and (methyl) acrylic acid
Material ratio.
Semi-finished product enter at the top of vacuum spraying absorption tower, deviate from ethylene oxide under vacuum condition on column plate, abjection finishes
Thick (methyl) hydroxy-ethyl acrylate through bottom of tower discharging pump, discharging condenser cooling, be sent into semi-finished product tank；The epoxy of tower top abjection
Ethane enters (methyl) acrylic acid material-compound tank after being absorbed via the extraction duct that (methyl) acrylic acid sprays.
Slightly (methyl) hydroxy-ethyl acrylate is delivered to progress short distance rectifying, short distance in short-path distillation kettle by pumping through semi-finished product tank
Three tunnels of distillation still discharge port point, bottom discharging is finished product, and the diameter first via is directly entered finished pot；Side discharge hole for discharge is raffinate,
It is beaten to a residual liquid tank through secondary route pump, is again introduced into short-path distillation kettle and carries out short distance rectifying；Go out again from short distance rectifying still
The secondary raffinate come is beaten to secondary residual liquid tank through third routing tail pump and is ready for distillation reaction.
Secondary raffinate after short-path distillation is beaten through pump to raffinate gravity tank, is flow automatically into distillation still by gravity tank and is steamed
It evaporates, gained product of distillation reenters a residual liquid tank after distillation, carries out short distance rectifying again；Short-path distillation and distillation follow successively
Ring carries out, and high level finished product is made, realizes continuous production.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (10)
1. a kind of continuous producing apparatus of (methyl) hydroxy-ethyl acrylate, which is characterized in that including material-compound tank, measuring tank, tubular type
Reactor, condenser, intermediate maturity tank, vacuum spraying absorption tower, short-path distillation kettle, finished pot and distillation still, (methyl) propylene
Acid, catalyst and polymerization inhibitor enter tubular reactor via material-compound tank, and ethylene oxide enters tubular reactor via measuring tank,
Ring-opening reaction is carried out in tubular reactor, and reaction mixture is made；Reaction mixture enters that condenser is condensed to isolate excess
Ethylene oxide and semi-finished product (methyl) hydroxy-ethyl acrylate, excess ethylene oxide return to measuring tank, semi-finished product (first from condenser
Base) hydroxy-ethyl acrylate enters intermediate maturity tank from condenser；Semi-finished product (methyl) hydroxy-ethyl acrylate from intermediate finished pot into
Enter vacuum spraying absorption tower, deviates from (methyl) acrylic acid, (methyl) acrylic acid of abjection from tower top under vacuum condition on column plate
Back to material-compound tank, deviates from thick (methyl) hydroxy-ethyl acrylate finished and be delivered to progress short distance essence in short-path distillation kettle from bottom of tower
It evaporates；Three tunnels of short-path distillation kettle discharge port point, the first via to finished pot, the second tunnel returns again to short-path distillation kettle；It is steamed again from short distance
It evaporates the raffinate that kettle comes out and enters distillation still progress distillation reaction through third road.
2. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that (methyl) third
Olefin(e) acid enters tubular reactor, canned motor pump tail via material-compound tank by canned motor pump, regulating valve, (methyl) acrylic acid mass flowmenter
Pipe is connected to material-compound tank to constitute (methyl) acrylic acid cycle；Ethylene oxide passes through metering pump, surge tank, epoxy second via measuring tank
Alkane mass flowmenter enters tubular reactor, and metering pump is connected to measuring tank to constitute ethylene oxide cycle.
3. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that in material-compound tank
If recycling water coil.
4. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that anti-in tubular type
It answers and sets thermometer on device and shell side recirculated water is chain.
5. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that centre at
Polymerization inhibitor is added in product tank.
6. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that intermediate maturity
Pot bottom sets sample tap.
7. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that abjection
(methyl) acrylic acid returns to material-compound tank after being absorbed via the extraction duct that (methyl) acrylic acid sprays；Deviate from the thick (first finished
Base) for hydroxy-ethyl acrylate through bottom of tower discharging pump, discharging condenser cooling, feeding semi-finished product tank is then sent to short-path distillation kettle
Carry out short distance rectifying.
8. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that short distance rectifying
Finished product and a raffinate are obtained afterwards, and three tunnels of short-path distillation kettle discharging point, the first via is from bottom discharge port to finished pot；Second road from
Kettle side discharge port returns again to short-path distillation kettle through a residual liquid tank and carries out short distance rectifying；The raffinate come out again from short-path distillation kettle
Secondary residual liquid tank is passed sequentially through from kettle side discharge port through third road, raffinate gravity tank enters distillation still and carries out distillation reaction.
9. the continuous producing apparatus of (methyl) hydroxy-ethyl acrylate according to claim 1, which is characterized in that distillation reaction
Gained product of distillation reenters a residual liquid tank afterwards, again returns to short-path distillation kettle and carries out short distance rectifying.
10. a kind of continuous producing apparatus using (methyl) hydroxy-ethyl acrylate described in any one of claim 1 to 9 produces
The method of (methyl) hydroxy-ethyl acrylate, which is characterized in that include the following steps：By (methyl) acrylic acid, catalyst and inhibition
Agent puts into tubular reactor via material-compound tank, ethylene oxide is put into tubular reactor via measuring tank, in tubular reactor
Ring-opening reaction is carried out, reaction mixture is made；Make reaction mixture enter condenser it is condensed isolate excess ethylene oxide and
Semi-finished product (methyl) hydroxy-ethyl acrylate, excess ethylene oxide return to measuring tank, semi-finished product (methyl) acrylic acid from condenser
Hydroxyl ethyl ester enters intermediate maturity tank from condenser；Polymerization inhibitor, semi-finished product (methyl) acrylic acid hydroxyl second are added into intermediate maturity tank
Ester enters vacuum spraying absorption tower from intermediate finished pot, deviates from (methyl) acrylic acid from tower top under vacuum condition on column plate, takes off
(methyl) acrylic acid gone out returns to material-compound tank, deviates from thick (methyl) hydroxy-ethyl acrylate finished and is delivered to short distance steaming from bottom of tower
Evaporate progress short distance rectifying in kettle；The discharging of short-path distillation kettle is finished product and a raffinate, and finished product to finished pot, one time raffinate enters one
Short-path distillation kettle is returned again to after secondary residual liquid tank and carries out short distance rectifying, obtains finished product and secondary raffinate, secondary raffinate pass sequentially through two
Secondary residual liquid tank, raffinate gravity tank enter distillation still and carry out distillation reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810058898.6A CN108383725A (en) | 2018-01-22 | 2018-01-22 | It is a kind of（Methyl）The continuous producing apparatus of hydroxy-ethyl acrylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810058898.6A CN108383725A (en) | 2018-01-22 | 2018-01-22 | It is a kind of（Methyl）The continuous producing apparatus of hydroxy-ethyl acrylate |
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| Publication Number | Publication Date |
|---|---|
| CN108383725A true CN108383725A (en) | 2018-08-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810058898.6A Withdrawn CN108383725A (en) | 2018-01-22 | 2018-01-22 | It is a kind of（Methyl）The continuous producing apparatus of hydroxy-ethyl acrylate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939774A (en) * | 2021-03-05 | 2021-06-11 | 武汉海翎化学工业有限公司 | Production method of methacrylic acid hydroxy ester or acrylic acid hydroxy ester |
| CN113912490A (en) * | 2020-09-29 | 2022-01-11 | 安徽联化新材料有限公司 | Preparation method and processing equipment of hydroxyethyl acrylate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524343A (en) * | 2013-09-27 | 2014-01-22 | 常州大学 | Method for synthesizing hydroxy-propyl acrylate |
| CN105272851A (en) * | 2014-07-14 | 2016-01-27 | 万华化学集团股份有限公司 | Preparation method of hydroxyethyl (meth)acrylate |
| CN105968011A (en) * | 2016-05-11 | 2016-09-28 | 常州海克莱化学有限公司 | Preparation technique of high-purity hydroxyethyl methacrylate |
-
2018
- 2018-01-22 CN CN201810058898.6A patent/CN108383725A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524343A (en) * | 2013-09-27 | 2014-01-22 | 常州大学 | Method for synthesizing hydroxy-propyl acrylate |
| CN105272851A (en) * | 2014-07-14 | 2016-01-27 | 万华化学集团股份有限公司 | Preparation method of hydroxyethyl (meth)acrylate |
| CN105968011A (en) * | 2016-05-11 | 2016-09-28 | 常州海克莱化学有限公司 | Preparation technique of high-purity hydroxyethyl methacrylate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912490A (en) * | 2020-09-29 | 2022-01-11 | 安徽联化新材料有限公司 | Preparation method and processing equipment of hydroxyethyl acrylate |
| CN112939774A (en) * | 2021-03-05 | 2021-06-11 | 武汉海翎化学工业有限公司 | Production method of methacrylic acid hydroxy ester or acrylic acid hydroxy ester |
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