CN107011165A - UV photo-curing monomer continuous production methods - Google Patents
UV photo-curing monomer continuous production methods Download PDFInfo
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- CN107011165A CN107011165A CN201710269333.8A CN201710269333A CN107011165A CN 107011165 A CN107011165 A CN 107011165A CN 201710269333 A CN201710269333 A CN 201710269333A CN 107011165 A CN107011165 A CN 107011165A
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- 239000000178 monomer Substances 0.000 title claims abstract description 30
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010924 continuous production Methods 0.000 title claims abstract description 11
- 230000032050 esterification Effects 0.000 claims abstract description 97
- 238000005886 esterification reaction Methods 0.000 claims abstract description 97
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 claims abstract description 35
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 199
- 239000000463 material Substances 0.000 claims description 114
- 238000005406 washing Methods 0.000 claims description 100
- 238000001556 precipitation Methods 0.000 claims description 86
- 239000002904 solvent Substances 0.000 claims description 77
- 239000007788 liquid Substances 0.000 claims description 69
- 239000012074 organic phase Substances 0.000 claims description 51
- 239000008346 aqueous phase Substances 0.000 claims description 45
- 239000003513 alkali Substances 0.000 claims description 42
- 239000000047 product Substances 0.000 claims description 42
- 238000004140 cleaning Methods 0.000 claims description 40
- 239000012043 crude product Substances 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 30
- 239000010408 film Substances 0.000 claims description 30
- 239000002244 precipitate Substances 0.000 claims description 29
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 26
- 238000007710 freezing Methods 0.000 claims description 26
- 230000008014 freezing Effects 0.000 claims description 26
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 18
- 238000006116 polymerization reaction Methods 0.000 claims description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 14
- 235000017550 sodium carbonate Nutrition 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000009833 condensation Methods 0.000 claims description 13
- 230000005494 condensation Effects 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 238000011084 recovery Methods 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 11
- 238000005086 pumping Methods 0.000 claims description 11
- 239000010409 thin film Substances 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 9
- 230000005484 gravity Effects 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 230000005764 inhibitory process Effects 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- 239000013557 residual solvent Substances 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 238000004807 desolvation Methods 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- 238000004148 unit process Methods 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims description 3
- 230000008016 vaporization Effects 0.000 claims description 3
- 238000004065 wastewater treatment Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000012374 esterification agent Substances 0.000 claims 1
- 239000004744 fabric Substances 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 238000000746 purification Methods 0.000 claims 1
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 230000007115 recruitment Effects 0.000 abstract description 2
- 150000007942 carboxylates Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 235000019628 coolness Nutrition 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000003613 toluenes Chemical class 0.000 description 2
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical class CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
- LJRSZGKUUZPHEB-UHFFFAOYSA-N 2-[2-(2-prop-2-enoyloxypropoxy)propoxy]propyl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COC(C)COC(=O)C=C LJRSZGKUUZPHEB-UHFFFAOYSA-N 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical class CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
Classifications
-
- 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)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of UV photo-curing monomers continuous production method, including the step such as esterification step, extract and separate, neutralization step, desolventizing process.The present invention improves the production capacity of UV photo-curing monomer wall scroll production lines, reduce the investment of unit production capacity, the consumption of raw material and power is reduced, reduces pollutant emission to improve the cleannes of production, shortens the reaction time, improve reaction efficiency, improve efficiency of post treatment, reduce and repeat recruitment, mitigate labor strength, realize Automatic Control, stable, raising product quality, device safety is improved, so as to improve every Technical and economical level.
Description
Technical field
The present invention relates to a kind of UV photo-curing monomers continuous production method.
Background technology
Existing UV photo-curing monomers（The esters of acrylic acid diluent of UV photocureable coating）Production technology be substantially all for
Batch (-type) mass production processes, wall scroll production line production capacity is small, specific productivity investment is high, material consumption and high energy consumption, use
Work is more, labor intensity is high, and concentration height, the flow of waste discharge are big, and reusable rate is low, is difficult realization and automatically controls, the production of production
Quality is unstable, and Technical and economical level has larger gap with the present invention.
The content of the invention
It is an object of the invention to provide a kind of production capacity of raising UV photo-curing monomer wall scroll production lines, unit is reduced
The investment of production capacity, reduces the consumption of raw material and power, reduces pollutant emission to improve the cleannes of production, when shortening reaction
Between, carry efficient UV photo-curing monomers continuous production method.
The present invention technical solution be：
A kind of UV photo-curing monomers continuous production method, it is characterized in that：Comprise the following steps：
（1）Esterification step
According to the UV photo-curing monomer kinds of required production, the desired amount of acrylic acid and corresponding polyalcohol and azeotropic dehydration will be calculated
Solvent, is respectively adopted and the first set reactor for being esterified production line is continuously added to after electronic flowmeter metering, automatic control flow
In, keep propylene excessive acid 5% or so；Meanwhile, esterification dehydration catalyst and polymerization inhibitor are also continuously added to be esterified production line
First set reactor in；
The esterification production line is in series by 3 to 6 " esterification units ", and each " esterification unit " staggered floor is arranged from high to low, by
Level is kept after this unit process kettle level stability from the potential difference between the reactor for flowing to next unit, adjacent esterification unit 1 to 2
Rice；
（2）Extract and separate, neutralization step
The esterification products that esterification step is sent continuously enter " washing extract and separate system ", with water by unreacted propylene in crude product
Acid elution is extracted into aqueous phase, and the organic matter isolated mutually continuously flows automatically to " in alkali cleaning and piece-rate system ", uses 5% soda ash solution
The acrylic acid of remaining is neutralized and washes aqueous phase, continuous self-flowing to " washing piece-rate system " again again for organic phase, and washing is except deentrainment
The impurity such as alkali, salt；
（3）Desolventizing process
The organic phase sent from extract and separate, neutralization step organic phase crude product groove with crude product transfering material pump first continuously enters " precipitation
Kettle group " carries out preliminary desolventizing, then with " thin film evaporator group " the UV photo-curing monomers of the most of solvent of preliminary removing are entered into one
Desolvation is walked, finally most of residual solvent is removed with " stripping tower group ", solvent is dropped to below 100ppm, obtain phase
The UV photo-curing monomer finished products answered；
" esterification unit ", using reaction kettle of the esterification as core, reactor upper side sets overfall；Each unit is by 1 esterification
Reactor, 1 set of acrylic acid recovery tower, the separator composition of 1 set of solvent and water azeotropic vaporization complete condenser, 1 set of solvent and water；It is described
Acrylic acid recovery tower is formed by connecting by the segregator on top and the board-like fractionating column of bottom, and 10 layers of griddle are set in board-like fractionating column
Plate tower tray, the liquid that segregator is condensed directly returns board-like fractionating column as the phegma of board-like fractionating column；
Reaction kettle of the esterification carries agitator and outer spiral heater, outer spiral heater water flowing steam heating；Reaction kettle of the esterification exists
Steamed while heating response containing solvent, water, acrylic acid steam, this steams top Steam Pipe of the vapour through reaction kettle of the esterification from plate
Board-like fractionating column is laterally entered below the basecoat tower tray of formula fractionating column, acrylic acid recovery tower is arranged on reaction kettle of the esterification
Face, from board-like Fractionator Bottom, flow back to reaction kettle of the esterification continues to participate in reaction to the liquid acrylic of recovery certainly, not in dephlegmator of top of the tower
The water and solvent vapo(u)r of condensation enter at the top of complete condenser from segregator upper end, and liquid is all condensed into complete condenser；Complete condenser
It is arranged in above separator, the solvent and water of condensation flow automatically to the middle part of separator from complete condenser bottom, by the close of solvent and water
Degree difference carries out Liquid liquid Separation；Separator is vertical type cylinder shape band inferior pyramidal structure, and separator is arranged higher than reaction kettle of the esterification, separation
The solvent that device upper side overfall continuous overflow goes out, all returns in reaction kettle of the esterification multiplexing, separator and is deposited to bottom
Water is by the continuous outer otherwise processed of discharge system after level stability in the liquid sealing pipe control separator of carry potential overflow function；Each esterification is single
The steam rates of the outer coil pipe heating of the reaction kettle of the esterification of member are controlled automatically according to the temperature of reaction solution in corresponding reaction kettle of the esterification
System；The cooling water flow of each set segregator is according to the temperature automatic control at the top of fractionating column；End set reaction kettle of the esterification continuous overflow
Go out esterification products, from esterification products material feeding cooling reactor is flowed into, material feeding cooling reactor chuck continuously leads to cooling water and is cooled to material in kettle
Esterification products in material feeding cooling reactor are continuously delivered to next procedure close to normal temperature, with esterification products pump and carried out at purifying by temperature
Reason.The regulation of esterification products pump frequency converter automatically controls output flow, keeps level stability in material feeding cooling reactor；
" the washing extract and separate system " is in series by multiple washing separative elements：Each unit by 1 washing stirred tank,
1 automatic water distributor, 1 water groove and 1 aqueous-phase material delivery pump composition, washing stirred tank is higher than automatic water distributor arrangement, water
Groove is arranged less than automatic water distributor；The front of advanced washing stirred tank of organic phase is mixed after washing with water, mixed liquor
From the outflow of washing stirred tank bottom, entered by gravity flow after level stability in liquid sealing pipe control washing stirred tank in automatic water distributor
Portion, organic phase floats to overflow behind top in automatic water distributor and gone under next unit, aqueous phase be deposited in automatic water distributor
Portion, is overflowed in water groove after controlling automatic water distributor level stability by liquid sealing pipe, and previous unit set is pumped with aqueous-phase material conveying
With or send outside system handle；The volume of washing stirred tank will meet organic phase and be mixed with water stop of the compound in washing stirred tank
Time is no less than 10 minutes；The volume of automatic water distributor is to meet the residence time of organic phase and aqueous-phase material in automatic water distributor
No less than half an hour；Staggered floor arranges that the potential difference between adjacent cells is at 2 meters or so, with reality to multistage washing separative element from high to low
Now flow automatically step by step；The photo-curing monomers of UV containing the solvent crude product that esterification products pumping comes first continuously enters the water of first washing separative element
Wash stirred tank, after from the water knockout drum of previous unit step by step from washing stirred tank, the automatic water distributor for flowing into next stage, then from final stage
Automatic water distributor] continuous overflow goes " in alkali cleaning and piece-rate system "；Washings used in final stage washing stirred tank from " washing again
The water groove of piece-rate system " is come with pumping, and the water feeding previous stage washing stirred tank of later stage water groove is applied mechanically, the 1st grade
Outside the water transmitting system of water groove, acrylic acid is gone together with the water that esterification is sent out；
Described " in alkali cleaning and piece-rate system " is single set washing piece-rate system, by 1 alkali cleaning stirred tank, 1 automatic segregator, 1
Platform aqueous-phase material groove and 1 aqueous-phase material delivery pump composition, alkali cleaning stirred tank arrange that aqueous-phase material groove is less than higher than automatic segregator
Automatic segregator is arranged；Front of organic phase continuously enters alkali cleaning stirred tank, the soda ash solution with being continuously added to alkali cleaning stirred tank
Mix and neutralize, gravity flow enters in the middle part of automatic segregator, organic phase floats to overflow behind top in automatic segregator and gone " again
Wash piece-rate system "；Aqueous phase is deposited to bottom, and aqueous-phase material groove is overflowed to after controlling automatic segregator level stability by liquid sealing pipe
In, with aqueous-phase material conveying pumping, out-of-bounds Waste Water Treatment goes processing to the brine waste in aqueous-phase material groove；Add alkali cleaning stirring
Acidity of the soda ash solution flow of kettle in alkali cleaning stirred tank is automatically controlled, to keep in alkali cleaning stirred tank material as neutrality；
The volume of alkali cleaning stirred tank will meet the residence time of organic phase and soda ash liquid mixture in alkali cleaning stirred tank no less than 10 points
Clock；The volume of separator is no less than half an hour to meet the residence time of organic phase and soda ash solution in automatic segregator；
Described " washing piece-rate system again " is single set washing piece-rate system, by 1 washing stirred tank, 1 automatic water distributor, 1
Water groove, 1 water delivery pump, 1 crude product groove, 1 crude product transfering material pump composition；Washing stirred tank is less than " in alkali cleaning and separating
The automatic segregator arrangement of system ", washing stirred tank arranges that water groove, crude product groove are less than automatic point higher than automatic water distributor
Hydrophone is arranged；Front of organic phase continuous stream is entered to wash stirred tank, continuous plus organic phase weight 1-3 fresh process water mixing
Agitator treating, enters in the middle part of automatic water distributor, organic phase is automatic by overflow after liquid sealing pipe control washing stirred tank level stability
Overflow behind top is floated in water knockout drum and removes crude product groove, continuously send " desolventizing process " to handle with crude product transfering material pump, crude product turns
The frequency converter regulation of material pump automatically controls output flow, keeps level stability in crude product groove；Aqueous phase is deposited to automatic water distributor
Bottom, is overflowed in water groove after controlling automatic water distributor level stability by liquid sealing pipe, and the water in water groove is conveyed with water and pumped
The final stage washing stirred tank of " washing extract and separate system " is applied mechanically；The volume of washing stirred tank will meet organic phase and be mixed with water conjunction
The thing residence time is no less than 10 minutes；The volume of automatic water distributor will meet organic phase and aqueous-phase material residence time no less than half
Hour.
" the precipitation kettle group " includes one-level precipitation kettle, two grades of precipitation kettles, just first de- recirculated water cooling condenser, de- freezing water coolings
Condenser, first desolventizing groove, first precipitate groove, first precipitate transfering material pump, first precipitation vavuum pump；One-level precipitation kettle and two grades
Precipitation kettle all carries in outer spiral heater, kettle and is equipped with rotary disc-type distributor, the agitating shaft by foreshortening to kettle internal upper part
Drive on the upside of rotation, disc type distributor outer provided with the baffle plate that 80 mm of circle are high, one is provided with baffle plate vertical direction middle and lower part
Enclose the mm of φ 6 hole；Pitch of holes is in 30mm；The organic phase that last process comes is continuously added in the middle part of the disk of one-level precipitation kettle, one-level
The material of precipitation bottom portion outflow is continuously added in the middle part of the disk of two grades of precipitation kettles；Add one-level precipitation kettle, two grades of precipitation kettles
Liquid is uniformly thrown to precipitation kettle wall by centrifugal force from disk side aperture, forms one layer of uniform falling liquid film, quickly steams solvent
Issue, after the Steam Pipe at the top of each kettle is discharged outside kettle, be combined into just de- recirculated water cooling condenser, first take off and freeze water condenser
The condenser group of series connection is condensed into liquid, and income just in desolventizing groove, returns esterification step multiplexing；Through just de- freezing water condenser
Freezing removes the tail gas after solvent and connects just precipitation vavuum pump from gas phase pipe, keeps system vacuum to be not less than 0.09MPa；One-level precipitation
Kettle and two grades of precipitation bottoms portion lead to a small amount of compressed air, to improve the polymerization inhibition effect of polymerization inhibitor in material；Enter one-level precipitation kettle and
The heating steam flow of the outer coil pipe of two grades of precipitation kettles or chuck is controlled according to the temperature automatic adjustment of respective bottom material, keeps one
Level precipitation kettle bottom temperature of charge is in 60 DEG C, two grades of precipitation kettle bottom temperature of charge at 80 DEG C；One-level precipitation kettle takes off higher than two grades
Molten kettle arrangement, two grades of precipitation kettles are arranged higher than first precipitate groove, to realize gravity flow；One-level precipitation kettle, two grades of precipitation bottoms portion
Material will flow out in time, keep basic no backup；The UV photo-curing monomers of the preliminary most of solvent of removing in first precipitate groove
" thin film evaporator group " further precipitation is sent with first precipitate transfering material pump；
" the thin film evaporator group " includes 1 scraper film evaporator, 1 recirculated water cooling condenser, 1 freezing water condensation
Device, 1 solvent groove, 1 precipitate groove, 1 precipitate transfering material pump, 1 set of Roots vacuum system；Scraper film evaporator
With outer coil pipe or sheathed heater；From " precipitation kettle group ", just precipitate transfering material pump supplied materials adds scraper film evaporator
Distributor, is scattered in one layer of thinner falling liquid film evenly in scraper film evaporator wall, quickly solvent is evaporated, from
The Steam Pipe discharge of scraper film evaporator, into recirculated water cooling condenser, the condenser group condensation of freezing water condenser series connection
Into liquid, take in solvent groove, return esterification step multiplexing；Chilled water condenser freezing removes the tail gas after solvent from gas phase pipe
Roots vacuum system is connect, keeps system vacuum to be not less than 0.095MPa；The logical a small amount of compression in scraper film evaporator bottom is empty
Gas, to improve the polymerization inhibition effect of polymerization inhibitor in material, enters the heating steam flow of the outer coil pipe of scraper film evaporator or chuck
According to the temperature automatic control of scraper film evaporator bottoms material, bottoms material temperature is kept to flow into precipitation at 80 DEG C or so
Thing groove, send " stripping tower group " to remove the solvent of remaining again with precipitate transfering material pump；
" the stripping tower group " includes one-level stripping tower, one-level transfering material pump, two grades of stripping towers, stripping recirculated water cooling condenser, strippings
Freeze water condenser, stripping solvent groove, finished product groove, finished product transfering material pump, stripping Roots vacuum system, air blower；One-level is blown
Liquid distribution trough and 10 meters or so high corrugated plate packing are all filled in de- tower, two grades of stripping towers；Precipitate transfering material pump supplied materials enters
Liquid distribution trough at the top of one-level stripping tower, the half air pumped in one-level stripping tower with air blower carries out solvent stripping,
The liquid that this strand of air enters in tower, one-level stripping tower on the downside of the packing section of one-level stripping tower is sent into from bottom with one-level transfering material pump
The liquid distribution trough on two grades of stripping tower top, second half air pumped in two grades of stripping towers with air blower carries out solvent and blown again
De-, the liquid that this strand of air enters in tower, two grades of stripping towers on the downside of the packing section of two grades of stripping towers flows into finished product groove from bottom
Warehouse for finished product is sent with finished product transfering material pump；Enter after discharging solvent-laden air, merging at the top of one-level stripping tower and two grades of stripping towers
Stripping recirculated water cooling condenser, the condenser group of stripping freezing water condenser series connection are condensed out in solvent liquid income solvent groove,
Esterification step multiplexing is returned, freeze the tail gas after water condenser freezing removes solvent through stripping connects stripping Roots vacuum machine from gas phase pipe
Group, keeps system vacuum to be not less than 0.095MPa.
The present invention improves the production capacity of UV photo-curing monomer wall scroll production lines, reduces the investment of unit production capacity, reduces former
The consumption of material and power, reduces pollutant emission to improve the cleannes of production, shortens the reaction time, improves reaction efficiency,
Raising efficiency of post treatment, reduces and repeats recruitment, mitigates labor strength, realizes Automatic Control, stable, raising product matter
Amount, improves device safety, so as to improve every Technical and economical level.Compared with the existing technology generally used, wall scroll
Production line production capacity can at least improve more than 2 times, can more to improve more than 5 times.Corresponding investment per unit capacity,
Having in terms of material consumption and energy consumption is significantly reduced, and can realize Automatic Control, and product quality and labor productivity are substantially carried
Height, single ton of production cost can decline nearly 1,000 yuan.
With reference to embodiment, the invention will be further described.
Embodiment
A kind of UV photo-curing monomers continuous production method, it is characterized in that：Comprise the following steps：
（1）Esterification step
According to the UV photo-curing monomer kinds of required production, the desired amount of acrylic acid and corresponding polyalcohol and azeotropic dehydration will be calculated
Solvent, is respectively adopted and the first set reactor for being esterified production line is continuously added to after electronic flowmeter metering, automatic control flow
In, keep propylene excessive acid 5% or so；Meanwhile, esterification dehydration catalyst and polymerization inhibitor are also continuously added to be esterified production line
First set reactor in；
The esterification production line is in series by 3 to 6 " esterification units ", and each " esterification unit " staggered floor is arranged from high to low, by
Level is kept after this unit process kettle level stability from the potential difference between the reactor for flowing to next unit, adjacent esterification unit 1 to 2
Rice；
（2）Extract and separate, neutralization step
The esterification products that esterification step is sent continuously enter " washing extract and separate system ", with water by unreacted propylene in crude product
Acid elution is extracted into aqueous phase, and the organic matter isolated mutually continuously flows automatically to " in alkali cleaning and piece-rate system ", uses 5% soda ash solution
The acrylic acid of remaining is neutralized and washes aqueous phase, continuous self-flowing to " washing piece-rate system " again again for organic phase, and washing is except deentrainment
The impurity such as alkali, salt；
（3）Desolventizing process
The organic phase sent from extract and separate, neutralization step organic phase crude product groove with crude product transfering material pump first continuously enters " precipitation
Kettle group " carries out preliminary desolventizing, then with " thin film evaporator group " the UV photo-curing monomers of the most of solvent of preliminary removing are entered into one
Desolvation is walked, finally most of residual solvent is removed with " stripping tower group ", solvent is dropped to below 100ppm, obtain phase
The UV photo-curing monomer finished products answered；
" esterification unit ", using reaction kettle of the esterification as core, reactor upper side sets overfall；Each unit is by 1 esterification
Reactor, 1 set of acrylic acid recovery tower, the separator composition of 1 set of solvent and water azeotropic vaporization complete condenser, 1 set of solvent and water；It is described
Acrylic acid recovery tower is formed by connecting by the segregator on top and the board-like fractionating column of bottom, and 10 layers of griddle are set in board-like fractionating column
Plate tower tray, the liquid that segregator is condensed directly returns board-like fractionating column as the phegma of board-like fractionating column；
Reaction kettle of the esterification carries agitator and outer spiral heater, outer spiral heater water flowing steam heating；Reaction kettle of the esterification exists
Steamed while heating response containing solvent, water, acrylic acid steam, this steams top Steam Pipe of the vapour through reaction kettle of the esterification from plate
Board-like fractionating column is laterally entered below the basecoat tower tray of formula fractionating column, acrylic acid recovery tower is arranged on reaction kettle of the esterification
Face, from board-like Fractionator Bottom, flow back to reaction kettle of the esterification continues to participate in reaction to the liquid acrylic of recovery certainly, not in dephlegmator of top of the tower
The water and solvent vapo(u)r of condensation enter at the top of complete condenser from segregator upper end, and liquid is all condensed into complete condenser；Complete condenser
It is arranged in above separator, the solvent and water of condensation flow automatically to the middle part of separator from complete condenser bottom, by the close of solvent and water
Degree difference carries out Liquid liquid Separation；Separator is vertical type cylinder shape band inferior pyramidal structure, and separator is arranged higher than reaction kettle of the esterification, separation
The solvent that device upper side overfall continuous overflow goes out, all returns in reaction kettle of the esterification multiplexing, separator and is deposited to bottom
Water is by the continuous outer otherwise processed of discharge system after level stability in the liquid sealing pipe control separator of carry potential overflow function；Each esterification is single
The steam rates of the outer coil pipe heating of the reaction kettle of the esterification of member are controlled automatically according to the temperature of reaction solution in corresponding reaction kettle of the esterification
System；The cooling water flow of each set segregator is according to the temperature automatic control at the top of fractionating column；End set reaction kettle of the esterification continuous overflow
Go out esterification products, from esterification products material feeding cooling reactor is flowed into, material feeding cooling reactor chuck continuously leads to cooling water and is cooled to material in kettle
Esterification products in material feeding cooling reactor are continuously delivered to next procedure close to normal temperature, with esterification products pump and carried out at purifying by temperature
Reason.The regulation of esterification products pump frequency converter automatically controls output flow, keeps level stability in material feeding cooling reactor；
" the washing extract and separate system " is in series by multiple washing separative elements：Each unit by 1 washing stirred tank,
1 automatic water distributor, 1 water groove and 1 aqueous-phase material delivery pump composition, washing stirred tank is higher than automatic water distributor arrangement, water
Groove is arranged less than automatic water distributor；The front of advanced washing stirred tank of organic phase is mixed after washing with water, mixed liquor
From the outflow of washing stirred tank bottom, entered by gravity flow after level stability in liquid sealing pipe control washing stirred tank in automatic water distributor
Portion, organic phase floats to overflow behind top in automatic water distributor and gone under next unit, aqueous phase be deposited in automatic water distributor
Portion, is overflowed in water groove after controlling automatic water distributor level stability by liquid sealing pipe, and previous unit set is pumped with aqueous-phase material conveying
With or send outside system handle；The volume of washing stirred tank will meet organic phase and be mixed with water stop of the compound in washing stirred tank
Time is no less than 10 minutes；The volume of automatic water distributor is to meet the residence time of organic phase and aqueous-phase material in automatic water distributor
No less than half an hour；Staggered floor arranges that the potential difference between adjacent cells is at 2 meters or so, with reality to multistage washing separative element from high to low
Now flow automatically step by step；The photo-curing monomers of UV containing the solvent crude product that esterification products pumping comes first continuously enters the water of first washing separative element
Wash stirred tank, after from the water knockout drum of previous unit step by step from washing stirred tank, the automatic water distributor for flowing into next stage, then from final stage
Automatic water distributor] continuous overflow goes " in alkali cleaning and piece-rate system "；Washings used in final stage washing stirred tank from " washing again
The water groove of piece-rate system " is come with pumping, and the water feeding previous stage washing stirred tank of later stage water groove is applied mechanically, the 1st grade
Outside the water transmitting system of water groove, acrylic acid is gone together with the water that esterification is sent out；
Described " in alkali cleaning and piece-rate system " is single set washing piece-rate system, by 1 alkali cleaning stirred tank, 1 automatic segregator, 1
Platform aqueous-phase material groove and 1 aqueous-phase material delivery pump composition, alkali cleaning stirred tank arrange that aqueous-phase material groove is less than higher than automatic segregator
Automatic segregator is arranged；Front of organic phase continuously enters alkali cleaning stirred tank, the soda ash solution with being continuously added to alkali cleaning stirred tank
Mix and neutralize, gravity flow enters in the middle part of automatic segregator, organic phase floats to overflow behind top in automatic segregator and gone " again
Wash piece-rate system "；Aqueous phase is deposited to bottom, and aqueous-phase material groove is overflowed to after controlling automatic segregator level stability by liquid sealing pipe
In, with aqueous-phase material conveying pumping, out-of-bounds Waste Water Treatment goes processing to the brine waste in aqueous-phase material groove；Add alkali cleaning stirring
Acidity of the soda ash solution flow of kettle in alkali cleaning stirred tank is automatically controlled, to keep in alkali cleaning stirred tank material as neutrality；
The volume of alkali cleaning stirred tank will meet the residence time of organic phase and soda ash liquid mixture in alkali cleaning stirred tank no less than 10 points
Clock；The volume of separator is no less than half an hour to meet the residence time of organic phase and soda ash solution in automatic segregator；
Described " washing piece-rate system again " is single set washing piece-rate system, by 1 washing stirred tank, 1 automatic water distributor, 1
Water groove, 1 water delivery pump, 1 crude product groove, 1 crude product transfering material pump composition；Washing stirred tank is less than " in alkali cleaning and separating
The automatic segregator arrangement of system ", washing stirred tank arranges that water groove, crude product groove are less than automatic point higher than automatic water distributor
Hydrophone is arranged；Front of organic phase continuous stream is entered to wash stirred tank, continuous plus organic phase weight 1-3 fresh process water mixing
Agitator treating, enters in the middle part of automatic water distributor, organic phase is automatic by overflow after liquid sealing pipe control washing stirred tank level stability
Overflow behind top is floated in water knockout drum and removes crude product groove, continuously send " desolventizing process " to handle with crude product transfering material pump, crude product turns
The frequency converter regulation of material pump automatically controls output flow, keeps level stability in crude product groove；Aqueous phase is deposited to automatic water distributor
Bottom, is overflowed in water groove after controlling automatic water distributor level stability by liquid sealing pipe, and the water in water groove is conveyed with water and pumped
The final stage washing stirred tank of " washing extract and separate system " is applied mechanically；The volume of washing stirred tank will meet organic phase and be mixed with water conjunction
The thing residence time is no less than 10 minutes；The volume of automatic water distributor will meet organic phase and aqueous-phase material residence time no less than half
Hour.
" the precipitation kettle group " includes one-level precipitation kettle, two grades of precipitation kettles, just first de- recirculated water cooling condenser, de- freezing water coolings
Condenser, first desolventizing groove, first precipitate groove, first precipitate transfering material pump, first precipitation vavuum pump；One-level precipitation kettle and two grades
Precipitation kettle all carries in outer spiral heater, kettle and is equipped with rotary disc-type distributor, the agitating shaft by foreshortening to kettle internal upper part
Drive on the upside of rotation, disc type distributor outer provided with the baffle plate that 80 mm of circle are high, one is provided with baffle plate vertical direction middle and lower part
Enclose the mm of φ 6 hole；Pitch of holes is in 30mm；The organic phase that last process comes is continuously added in the middle part of the disk of one-level precipitation kettle, one-level
The material of precipitation bottom portion outflow is continuously added in the middle part of the disk of two grades of precipitation kettles；Add one-level precipitation kettle, two grades of precipitation kettles
Liquid is uniformly thrown to precipitation kettle wall by centrifugal force from disk side aperture, forms one layer of uniform falling liquid film, quickly steams solvent
Issue, after the Steam Pipe at the top of each kettle is discharged outside kettle, be combined into just de- recirculated water cooling condenser, first take off and freeze water condenser
The condenser group of series connection is condensed into liquid, and income just in desolventizing groove, returns esterification step multiplexing；Through just de- freezing water condenser
Freezing removes the tail gas after solvent and connects just precipitation vavuum pump from gas phase pipe, keeps system vacuum to be not less than 0.09MPa；One-level precipitation
Kettle and two grades of precipitation bottoms portion lead to a small amount of compressed air, to improve the polymerization inhibition effect of polymerization inhibitor in material；Enter one-level precipitation kettle and
The heating steam flow of the outer coil pipe of two grades of precipitation kettles or chuck is controlled according to the temperature automatic adjustment of respective bottom material, keeps one
Level precipitation kettle bottom temperature of charge is in 60 DEG C, two grades of precipitation kettle bottom temperature of charge at 80 DEG C；One-level precipitation kettle takes off higher than two grades
Molten kettle arrangement, two grades of precipitation kettles are arranged higher than first precipitate groove, to realize gravity flow；One-level precipitation kettle, two grades of precipitation bottoms portion
Material will flow out in time, keep basic no backup；The UV photo-curing monomers of the preliminary most of solvent of removing in first precipitate groove
" thin film evaporator group " further precipitation is sent with first precipitate transfering material pump；
" the thin film evaporator group " includes 1 scraper film evaporator, 1 recirculated water cooling condenser, 1 freezing water condensation
Device, 1 solvent groove, 1 precipitate groove, 1 precipitate transfering material pump, 1 set of Roots vacuum system；Scraper film evaporator
With outer coil pipe or sheathed heater；From " precipitation kettle group ", just precipitate transfering material pump supplied materials adds scraper film evaporator
Distributor, is scattered in one layer of thinner falling liquid film evenly in scraper film evaporator wall, quickly solvent is evaporated, from
The Steam Pipe discharge of scraper film evaporator, into recirculated water cooling condenser, the condenser group condensation of freezing water condenser series connection
Into liquid, take in solvent groove, return esterification step multiplexing；Chilled water condenser freezing removes the tail gas after solvent from gas phase pipe
Roots vacuum system is connect, keeps system vacuum to be not less than 0.095MPa；The logical a small amount of compression in scraper film evaporator bottom is empty
Gas, to improve the polymerization inhibition effect of polymerization inhibitor in material, enters the heating steam flow of the outer coil pipe of scraper film evaporator or chuck
According to the temperature automatic control of scraper film evaporator bottoms material, bottoms material temperature is kept to flow into precipitation at 80 DEG C or so
Thing groove, send " stripping tower group " to remove the solvent of remaining again with precipitate transfering material pump；
" the stripping tower group " includes one-level stripping tower, one-level transfering material pump, two grades of stripping towers, stripping recirculated water cooling condenser, strippings
Freeze water condenser, stripping solvent groove, finished product groove, finished product transfering material pump, stripping Roots vacuum system, air blower；One-level is blown
Liquid distribution trough and 10 meters or so high corrugated plate packing are all filled in de- tower, two grades of stripping towers；Precipitate transfering material pump supplied materials enters
Liquid distribution trough at the top of one-level stripping tower, the half air pumped in one-level stripping tower with air blower carries out solvent stripping,
The liquid that this strand of air enters in tower, one-level stripping tower on the downside of the packing section of one-level stripping tower is sent into from bottom with one-level transfering material pump
The liquid distribution trough on two grades of stripping tower top, second half air pumped in two grades of stripping towers with air blower carries out solvent and blown again
De-, the liquid that this strand of air enters in tower, two grades of stripping towers on the downside of the packing section of two grades of stripping towers flows into finished product groove from bottom
Warehouse for finished product is sent with finished product transfering material pump；Enter after discharging solvent-laden air, merging at the top of one-level stripping tower and two grades of stripping towers
Stripping recirculated water cooling condenser, the condenser group of stripping freezing water condenser series connection are condensed out in solvent liquid income solvent groove,
Esterification step multiplexing is returned, freeze the tail gas after water condenser freezing removes solvent through stripping connects stripping Roots vacuum machine from gas phase pipe
Group, keeps system vacuum to be not less than 0.095MPa.
Application examples 1：
Per hour by the auxiliary agent such as 1.26 tons of acrylic acid, 1.6 tons of tripropylene glycols, 3.3 tons of solvent toluenes and catalyst, polymerization inhibitor
It is continuously added to be covered in reactor for the esterification production line head that 4 esterification units of core are connected by 4 20 m3 reaction kettle of the esterification,
End set reactor can be exported continuously containing 20000 tons of TPGDA（Tri (propylene glycol) diacrylate）Carboxylate.Carboxylate passes through
By 3 washing separative elements（Per unit containing 1 10m3 washings stirred tank, 1 40 m3 automatic water distributors, 15 m3 water groove）
" the washing extract and separate system " being in series carries out washing extraction processing；By by 1 10 m3 alkali cleanings stirred tank, 1 40
M3 automatic segregators, " in alkali cleaning and the piece-rate system " of 15 m3 neutralizers grooves composition carry out neutralisation treatment；By by 1
What 10 m3 washings stirred tank, 1 40 m3 automatic water distributors, 15 m3 water groove, 15 m3 crude products groove were constituted " washes again
Piece-rate system " carries out washing process again；By tentatively de- for " the precipitation kettle group " of core by two precipitation kettles of φ 1500 × 2500
It is molten；By by " thin film evaporator group " the further precipitation of a 4 m2 scraper film evaporators for core；Pass through two again
The stripping towers of φ 900 fall most of residual solvents for " stripping tower group " stripping of core, and 20000 tons of solvents are produced every year
TPGDA less than 100ppm.
Application examples 2：By 958 kilograms of acrylic acid, 566 kilograms of trimethylolpropanes, 1.26 tons of solvent toluenes and urge per hour
The auxiliary agents such as agent, polymerization inhibitor are continuously added to the esterification life connected by 4 10 m3 reaction kettle of the esterification for 4 esterification units of core
In producing line head set reactors, end set reactor can be exported continuously containing 10000 tons of TMPTA（Trimethylolpropane trimethacrylate）'s
Carboxylate.Carboxylate passes through by 3 washing separative elements（Divide water automatically containing 15 m3 washings stirred tank, 1 20 m3 per unit
Device, 12 m3 water groove）" the washing extract and separate system " being in series carries out washing extraction processing；By by 15 m3
Alkali cleaning stirred tank, 1 20 m3 automatic segregators, " in alkali cleaning and the piece-rate system " of 12 m3 neutralizers grooves composition are carried out
Neutralisation treatment；By washing stirred tank, 1 20 m3 automatic water distributors, 12 m3 water groove, 12 m3 crude product by 15 m3
" washing piece-rate system again " of groove composition carries out washing process again；By being core by two precipitation kettles of φ 1200 × 2500
" precipitation kettle group " preliminary precipitation；By entering one by a 2 m2 scraper film evaporators for " the thin film evaporator group " of core
Walk precipitation；Fall most of residual solvents by two stripping towers of φ 700 for " stripping tower group " stripping of core again, annual production
Go out the TMPTA that 10000 tons of solvents are less than 100ppm.
Claims (4)
1. a kind of UV photo-curing monomers continuous production method, it is characterized in that：Comprise the following steps：
（1）Esterification step
According to the UV photo-curing monomer kinds of required production, the desired amount of acrylic acid and corresponding polyalcohol and azeotropic dehydration will be calculated
Solvent, is continuously added to be esterified in the first set reactor of production line；Meanwhile, by esterification dehydration catalyst and polymerization inhibitor
It is continuously added to be esterified in the first set reactor of production line；
The esterification production line is in series by 3 to 6 " esterification units ", and each " esterification unit " staggered floor is arranged from high to low, by
Level is kept after this unit process kettle level stability from the potential difference between the reactor for flowing to next unit, adjacent esterification unit 1 to 2
Rice；
（2）Extract and separate, neutralization step
The esterification products that esterification step is sent continuously enter " washing extract and separate system ", with water by unreacted propylene in crude product
Acid elution is extracted into aqueous phase, and the organic matter isolated mutually continuously flows automatically to " in alkali cleaning and piece-rate system ", will with soda ash solution
The acrylic acid of remaining, which is neutralized, washes aqueous phase, and continuous self-flowing, to " washing piece-rate system again ", washs and remove the miscellaneous of deentrainment organic phase again
Matter；
（3）Desolventizing process
The organic phase sent from extract and separate, neutralization step organic phase crude product groove with crude product transfering material pump first continuously enters " precipitation
Kettle group " carries out preliminary desolventizing, then with " thin film evaporator group " the UV photo-curing monomers of the most of solvent of preliminary removing are entered into one
Desolvation is walked, finally most of residual solvent is removed with " stripping tower group ", solvent is dropped to below 100ppm, obtain phase
The UV photo-curing monomer finished products answered.
2. UV photo-curing monomers continuous production method according to claim 1, it is characterized in that：" esterification unit " with
Reaction kettle of the esterification is core, and reactor upper side sets overfall；Each unit includes 1 reaction kettle of the esterification, 1 set of acrylic acid and returned
Receive the separator of tower, 1 set of solvent and water azeotropic vaporization complete condenser, 1 set of solvent and water；The acrylic acid recovery tower is divided by top
Condenser and the board-like fractionating column of bottom are formed by connecting, and 10 layers of macroporous plate tower tray, the liquid of segregator condensation are set in board-like fractionating column
Body directly returns board-like fractionating column as the phegma of board-like fractionating column；
Reaction kettle of the esterification carries agitator and outer spiral heater, outer spiral heater water flowing steam heating；Reaction kettle of the esterification exists
Steamed while heating response containing solvent, water, acrylic acid steam, this steams top Steam Pipe of the vapour through reaction kettle of the esterification from plate
Board-like fractionating column is laterally entered below the basecoat tower tray of formula fractionating column, acrylic acid recovery tower is arranged on reaction kettle of the esterification
Face, from board-like Fractionator Bottom, flow back to reaction kettle of the esterification continues to participate in reaction to the liquid acrylic of recovery certainly, not in dephlegmator of top of the tower
The water and solvent vapo(u)r of condensation enter at the top of complete condenser from segregator upper end, and liquid is all condensed into complete condenser；Complete condenser
It is arranged in above separator, the solvent and water of condensation flow automatically to the middle part of separator from complete condenser bottom, by the close of solvent and water
Degree difference carries out Liquid liquid Separation；Separator arranges that it is molten that separator upper side overfall continuous overflow goes out higher than reaction kettle of the esterification
Agent, all returns to the liquid sealing pipe control separation that the water of bottom is deposited in reaction kettle of the esterification multiplexing, separator by carry potential overflow function
The outer otherwise processed of continuous discharge system after level stability in device；End set reaction kettle of the esterification continuous overflow goes out esterification products, from inflow
Esterification products material feeding cooling reactor, material feeding cooling reactor chuck continuously leads to cooling water and is cooled to temperature of charge in kettle and, close to normal temperature, uses ester
Change product pump and the esterification products in material feeding cooling reactor are continuously delivered into next procedure progress purification process.
3. UV photo-curing monomers continuous production method according to claim 1, it is characterized in that：" the washing extraction point
From system " it is in series by multiple washing separative elements：Each unit is by 1 washing stirred tank, 1 automatic water distributor, 1 water
Groove and 1 aqueous-phase material delivery pump composition, washing stirred tank arrange that water groove is less than automatic water distributor cloth higher than automatic water distributor
Put；The advanced stirred tank of washing of front of organic phase is mixed after washing with water, and mixed liquor flows out from washing stirred tank bottom,
Entered by gravity flow after level stability in liquid sealing pipe control washing stirred tank in the middle part of automatic water distributor, organic phase is in automatic water distributor
In float to overflow behind top and remove next unit, aqueous phase is deposited to bottom in automatic water distributor, by automatic point of liquid sealing pipe control
Overflowed to after hydrophone level stability in water groove, pumping previous unit with aqueous-phase material conveying applies mechanically or send processing outside system；Washing
The volume of stirred tank will meet organic phase and be mixed with water residence time of the compound in washing stirred tank no less than 10 minutes；Automatically
The volume of water knockout drum is no less than half an hour to meet the residence time of organic phase and aqueous-phase material in automatic water distributor；Multistage washing
Separative element from high to low arrange by staggered floor, is flow automatically step by step with realizing；The photo-curing monomers of UV containing solvent that esterification products pumping comes are thick
Product first continuously enter the washing stirred tank of first washing separative element, after from the water knockout drum of previous unit step by step from flowing into next stage
Stirred tank, automatic water distributor are washed, then from the automatic water distributor of final stage] continuous overflow goes " in alkali cleaning and piece-rate system "；Final stage
Washings used in washing stirred tank are come from the water groove of " washing piece-rate system again " with pumping, the water of later stage water groove
Feeding previous stage washing stirred tank is applied mechanically, and outside the water transmitting system of the 1st grade of water groove, recovery third is gone together with the water that esterification is sent out
Olefin(e) acid；
Described " in alkali cleaning and piece-rate system " is single set washing piece-rate system, by 1 alkali cleaning stirred tank, 1 automatic segregator, 1
Platform aqueous-phase material groove and 1 aqueous-phase material delivery pump composition, alkali cleaning stirred tank arrange that aqueous-phase material groove is less than higher than automatic segregator
Automatic segregator is arranged；Front of organic phase continuously enters alkali cleaning stirred tank, the soda ash solution with being continuously added to alkali cleaning stirred tank
Mix and neutralize, gravity flow enters in the middle part of automatic segregator, organic phase floats to overflow behind top in automatic segregator and gone " again
Wash piece-rate system "；Aqueous phase is deposited to bottom, and aqueous-phase material groove is overflowed to after controlling automatic segregator level stability by liquid sealing pipe
In, with aqueous-phase material conveying pumping, out-of-bounds Waste Water Treatment goes processing to the brine waste in aqueous-phase material groove；Alkali cleaning stirred tank
Volume will meet the residence time of organic phase and soda ash liquid mixture in alkali cleaning stirred tank no less than 10 minutes；The body of separator
Product is no less than half an hour to meet the residence time of organic phase and soda ash solution in automatic segregator；
Described " washing piece-rate system again " washs piece-rate system, including 1 washing stirred tank, 1 automatic water distributor, 1 for single set
Platform water groove, 1 water delivery pump, 1 crude product groove, 1 crude product transfering material pump；Stirred tank is washed less than " in alkali cleaning and segregative line
The automatic segregator arrangement of system ", washing stirred tank arranges that water groove, crude product groove are less than point water automatically higher than automatic water distributor
Device is arranged；Front of organic phase continuous stream is entered to wash stirred tank, and continuous plus organic phase weight 1-3 fresh process water mixing is stirred
Washing is mixed, is entered by overflow after liquid sealing pipe control washing stirred tank level stability in the middle part of automatic water distributor, organic phase is being divided automatically
Overflow behind top is floated in hydrophone and removes crude product groove, continuously send " desolventizing process " to handle with crude product transfering material pump, crude product turns material
The regulation of pump frequency converter automatically controls output flow, keeps level stability in crude product groove；Aqueous phase is deposited under automatic water distributor
Portion, is overflowed in water groove after controlling automatic water distributor level stability by liquid sealing pipe, the water conveying pumping " water of the water in water groove
Wash extract and separate system " final stage washing stirred tank apply mechanically；The volume of washing stirred tank will meet organic phase and be mixed with water compound
Residence time is no less than 10 minutes；It is small no less than half that the volume of automatic water distributor will meet organic phase and aqueous-phase material residence time
When.
4. UV photo-curing monomers continuous production method according to claim 1, it is characterized in that：" the precipitation kettle group "
Including one-level precipitation kettle, just two grades of precipitation kettles, de- recirculated water cooling condenser, just de- freezing water condenser, first desolventizing groove, just de-
Molten thing groove, first precipitate transfering material pump, first precipitation vavuum pump；One-level precipitation kettle and two grades of precipitation kettles are all heated with outer coil pipe
Rotary disc-type distributor is equipped with device, kettle, is rotated by foreshortening to the agitating shaft of kettle internal upper part and driving, outside disc type distributor
Along upside provided with a circle baffle plate, a collar aperture is provided with baffle plate vertical direction middle and lower part；The organic phase that last process comes is continuously added to
In the middle part of the disk of one-level precipitation kettle, the material of one-level precipitation bottom portion outflow is continuously added in the middle part of the disk of two grades of precipitation kettles；Plus
Enter one-level precipitation kettle, the liquid of two grades of precipitation kettles and be uniformly thrown to precipitation kettle wall from disk side aperture by centrifugal force, form one
Solvent, is quickly evaporated by the uniform falling liquid film of layer, after the Steam Pipe at the top of each kettle is discharged outside kettle, is combined into just de- circulation
Water condenser, the condenser group of just de- freezing water condenser series connection are condensed into liquid, and income just in desolventizing groove, returns esterification work
Sequence is multiplexed；Tail gas after removing solvent through just de- freezing water condenser freezing connects just precipitation vavuum pump from gas phase pipe, keeps system true
Reciprocal of duty cycle is not less than 0.09MPa；One-level precipitation kettle and two grades of precipitation bottoms portion lead to a small amount of compressed air, to improve polymerization inhibitor in material
Polymerization inhibition effect；Keep one-level precipitation kettle bottom temperature of charge in 60 DEG C, two grades of precipitation kettle bottom temperature of charge at 80 DEG C；One
Higher than two grades precipitation kettle arrangements of level precipitation kettle, two grades of precipitation kettles are arranged higher than first precipitate groove, to realize gravity flow；One-level precipitation
Kettle, two grades of precipitation kettle bottoms materials will flow out in time, keep basic no backup；Preliminary removing is most of molten in first precipitate groove
The UV photo-curing monomers of agent send " thin film evaporator group " further precipitation with first precipitate transfering material pump；
" the thin film evaporator group " includes 1 scraper film evaporator, 1 recirculated water cooling condenser, 1 freezing water condensation
Device, 1 solvent groove, 1 precipitate groove, 1 precipitate transfering material pump, 1 set of Roots vacuum system；Scraper film evaporator
With outer coil pipe or sheathed heater；From " precipitation kettle group ", just precipitate transfering material pump supplied materials adds scraper film evaporator
Distributor, is scattered in one layer of thinner falling liquid film evenly in scraper film evaporator wall, quickly solvent is evaporated, from
The Steam Pipe discharge of scraper film evaporator, into recirculated water cooling condenser, the condenser group condensation of freezing water condenser series connection
Into liquid, take in solvent groove, return esterification step multiplexing；Chilled water condenser freezing removes the tail gas after solvent from gas phase pipe
Roots vacuum system is connect, keeps system vacuum to be not less than 0.095MPa；The logical a small amount of compression in scraper film evaporator bottom is empty
Gas, to improve the polymerization inhibition effect of polymerization inhibitor in material, send " stripping tower group " to remove the solvent of remaining again with precipitate transfering material pump；
" the stripping tower group " includes one-level stripping tower, one-level transfering material pump, two grades of stripping towers, stripping recirculated water cooling condenser, strippings
Freeze water condenser, stripping solvent groove, finished product groove, finished product transfering material pump, stripping Roots vacuum system, air blower；One-level is blown
Liquid distribution trough and corrugated plate packing are all filled in de- tower, two grades of stripping towers；Precipitate transfering material pump supplied materials enters one-level stripping tower top
The liquid distribution trough in portion, the half air pumped in one-level stripping tower with air blower carries out solvent stripping, and this strand of air is from one
Enter the liquid in tower, one-level stripping tower on the downside of the packing section of level stripping tower to be sent on two grades of stripping towers with one-level transfering material pump from bottom
The liquid distribution trough in portion, second half air pumped in two grades of stripping towers with air blower carries out solvent stripping again, this strand of air
The liquid entered on the downside of the packing section of two grades of stripping towers in tower, two grades of stripping towers flows into finished product groove finished product transfering material pump from bottom
Send warehouse for finished product；Solvent-laden air is discharged at the top of one-level stripping tower and two grades of stripping towers, stripping recirculated water cooling is entered after merging
Condenser, the condenser group of stripping freezing water condenser series connection are condensed out in solvent liquid income solvent groove, are returned esterification step and are answered
With the tail gas after removing solvent through stripping freezing water condenser freezing connects stripping Roots vacuum system from gas phase pipe, keeps system true
Reciprocal of duty cycle is not less than 0.095MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108129267A (en) * | 2018-01-11 | 2018-06-08 | 吉林凯莱英医药化学有限公司 | Low temperature Total continuity reaction system and application |
| CN110684470A (en) * | 2019-10-21 | 2020-01-14 | 江苏利田科技股份有限公司 | Method for preparing acrylate adhesive by using UV monomer wastewater and acrylate adhesive |
| CN110683950A (en) * | 2019-10-21 | 2020-01-14 | 江苏利田科技股份有限公司 | Method and device for recycling UV (ultraviolet) photocuring monomer catalyst, polymerization inhibitor, reducing agent and decoloring agent |
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| US20080015384A1 (en) * | 2006-07-11 | 2008-01-17 | Hidefumi Haramaki | Process for producing acrylic ester |
| CN101041621A (en) * | 2006-11-24 | 2007-09-26 | 中国石油集团工程设计有限责任公司东北分公司 | Method for preparing (methyl) butyl acrylate |
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| CN108129267A (en) * | 2018-01-11 | 2018-06-08 | 吉林凯莱英医药化学有限公司 | Low temperature Total continuity reaction system and application |
| CN108129267B (en) * | 2018-01-11 | 2024-04-19 | 吉林凯莱英医药化学有限公司 | Low-temperature full-continuous reaction system and application |
| CN110684470A (en) * | 2019-10-21 | 2020-01-14 | 江苏利田科技股份有限公司 | Method for preparing acrylate adhesive by using UV monomer wastewater and acrylate adhesive |
| CN110683950A (en) * | 2019-10-21 | 2020-01-14 | 江苏利田科技股份有限公司 | Method and device for recycling UV (ultraviolet) photocuring monomer catalyst, polymerization inhibitor, reducing agent and decoloring agent |
| CN110684470B (en) * | 2019-10-21 | 2022-03-01 | 江苏利田科技股份有限公司 | Method for preparing acrylate adhesive by using UV monomer wastewater and acrylate adhesive |
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