CN106478584B - The control method of ethylene carbonate synthesis technology - Google Patents
The control method of ethylene carbonate synthesis technology Download PDFInfo
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- CN106478584B CN106478584B CN201510540800.7A CN201510540800A CN106478584B CN 106478584 B CN106478584 B CN 106478584B CN 201510540800 A CN201510540800 A CN 201510540800A CN 106478584 B CN106478584 B CN 106478584B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
- C07D317/38—Ethylene carbonate
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Abstract
The present invention relates to a kind of control method of ethylene carbonate synthesis technology, ethylene carbonate is generated using carbon dioxide and ethylene oxide gas-liquid-solid reaction, mainly solves easy temperature runaway existing in the prior art, the problems such as product purity is lower.The present invention controls the critical process Con trolling index of the reaction by automatic control system, catalyst is fixed in reactor bed using perforated baffle, liquid and gas raw material enters from reactor upper and lower part respectively, one section of synthesis reactor liquid level is controlled using one section of synthesis reactor outlet liquid phase produced quantity, utilize the technical solution of second stage reactor outlet liquid phase produced quantity control product purity, it preferably solves the problems, such as this, can be used for the industrialized production of ethylene carbonate Lipase absobed.
Description
Technical field
The present invention relates to a kind of control methods of ethylene carbonate synthesis technology, and specially one kind is by ethylene oxide and dioxy
Change the control method that carbon catalysis generates ethylene carbonate synthesis technology.
Background technique
Ethylene carbonate (EC) is a kind of excellent polar high-boiling solvent and important organic synthesis raw material.20th century are later half
Phase, various countries researcher have carried out numerous research, many new synthesis technologies and new catalyst quilt to the synthesis of carbonic ester
It was found that.EC traditional production method is phosgenation, but its there are process flows it is long, yield is low, at high cost the disadvantages of, and phosgene
Toxicity is big, seriously polluted, has substantially stopped using in developed country.With CO2It is that raw material direct esterification prepares carbonic acid with EO
Vinyl acetate is a kind of efficient, green, environmentally friendly synthesis new intermediate ester method, and provides a chemical utilization two
The new way for aoxidizing carbon resource, can receive apparent economic benefit and social benefit, by various countries' most attention, be suitble to extensive
Industrialized production.
EO and CO2In reaction process, CO2For nonpolar molecule, there is faintly acid, proton can be provided.Parent of the EO in nucleopilic reagent
Under nuclear attack, nucleophilic addition can occur, open loop obtains addition product.CO2Reaction with EO is nucleophilic addition, by nucleophilic plus
It is reacted at reaction mechanism, catalyst is as nucleopilic reagent.
The method majority of production cyclic carbonate reported at present is using Lewis acid metal compound and Lewis alkali
The binary homogeneous catalyst of composition, used in Lewis acid metal compound include alkali (soil) metal halide, transition metal
Salt, transition metal or Main group metal complexes, used Lewis alkali have organic base (such as DMF, DMAP etc.), quaternary ammonium salt, quaternary phosphine
Salt, imidazole salts, crown ether etc..Perhaps activity, selectivity be not high for these catalyst systems, or has used toxicity very strong organic molten
Agent, and homogeneous catalysis system there are catalyst to be difficult to the shortcomings that separating.And more heterogeneous catalysis system packet is used at present
Include metal oxide system (such as CeO2-ZrO2, Green Chem.2004,6,206-214), basic zeolite system (such as Cs/KX,
J.Catal.2001,199,85-91) etc., these active catalyst systems are low, and the required reaction time is longer.Xia Chungu etc.
By ZnCl2It is immobilized on chitin carrier, although achieving higher catalytic activity, activity drop after catalyst is applied 5 times
Low about 8%, thus it is speculated that the possible reason is the loss (Appl.Catal.A 2005,279,125- of catalyst activity component
129).Therefore, develop it is a kind of it is easily separated, active it is high, reaction condition is mild, the catalyst system of easy in inactivation does not seem particularly significant.
CN1421431A discloses ethylene glycol and urea in the presence of solid base catalyst, in the item for depressurizing or rousing nitrogen
Reaction generates ethylene carbonate under part, though technique selectivity is high, reaction condition is mild, it is with ethylene glycol and urea for original
Material, other than obtaining reaction product ethylene carbonate, while can also generate ammonia, and meeting environment pollutes, and improve environmental protection
Cost.
CN85100162A discloses a kind of process for synthesising vinylcarbonate by complex catalyst, to the high pressure for having electromagnetic agitation
Catalyst and ethylene oxide are added in kettle, is passed through CO2To 6atm, heated in bath of draining the oil, pressure first rises and reduces afterwards in kettle, reduces
Then continue to be passed through CO afterwards2, it is maintained at pressure in the range of 20-25atm, reaction is accused when confirming that pressure no longer reduces in kettle
It completes, after logical cooling water is cooled to room temperature, takes out white solid in kettle, the carbon of 99.9% yield (to ethylene oxide) can be obtained
Vinyl acetate.Though the technique process is simple, high income, complicated for operation, it is difficult to control, is not suitable for industrialized production.
CN101838257A discloses a kind of method for preparing ethylene carbonate, the admixture of gas that ethylene is obtained
In ethylene oxide and carbon dioxide absorption into ethylene carbonate ester solution, in the presence of a catalyst, the epoxy second in solution
Alkane and carbon dioxide reaction prepare ethylene carbonate, and unreacted carbon dioxide recycle is into reaction system.This method operation letter
Single, low energy consumption, but there are EO conversion ratio is low, reacts the problems such as incomplete.
Summary of the invention
The technical problem to be solved by the present invention is to existing ethylene carbonate synthesis technology, there are following critical issues, first is that
Since exothermic heat of reaction amount is big, the fluctuation of outer circulation amount easily causes bed temperature runaway；Second is that level fluctuation easily causes epoxy in reactor
The residence time is insufficient in the reactor for ethane, causes product purity lower；Third is that gas, which enters circulating pump easily, makes internal circulating load moment
It reduces, causes reactor temperature runaway.And in existing literature and data few corresponding control methods report.The present invention by using
A kind of control method of new ethylene carbonate synthesis technology, preferably solves the problems, such as this, this method can be applied to industrial life
In production.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows: a kind of ethylene carbonate synthesis technology
Control method, the synthesis of ethylene carbonate include one section of synthesis reactor (1), circulating pump surge tank (3), circulating pump (4), circulation
Cooler (2), two sections of synthesis reactor (5), product pump surge tank (8), product pump (6) and EO tourie (7)；Ethylene oxide is former
Expect that (S.1) and carbon dioxide raw material (S.2) after the reaction of one section of synthesis reactor and two sections of synthesis reactor, obtain carbonic acid
Vinyl acetate product (S.17)；It is characterized in that one section of synthesis reactor catalyst bed temperature rise is by one section of synthesis reactor outer circulation
Control valve (V.1) control；Ethylene carbonate product purity is by two sections of synthesis reactor extraction control valve (V.6) controls.
In above-mentioned technical proposal, it is preferable that the synthesis technology of ethylene carbonate the following steps are included:
I) ethylene oxide raw material (S.1) and one section of synthesis reactor feed carbon dioxide (S.4) respectively enter a Duan Hecheng
The upper and lower part of reactor (1), and react in the reactor；
Ii) reaction obtains in one section of synthesis reactor (1) liquid outlet stream (S.6) and unreacted gas vent
Logistics (S.5) is flowed out by the bottom and top of reactor respectively；Liquid outlet stream enters circulating pump surge tank (3), separates
To circulating pump surge tank liquid phase exit stream (S.9) obtain after circulating pump (4) are pressurized and recirculation cooler (2) is cooling
Circulation logistics (S.11) is back to one section of synthesis reactor liquid phase entrance, remaining is as two sections of synthesis reactor liquid phase feedings
(S.12) enter two sections of synthesis reactor (5) tops；
Iii) two sections of synthesis reactor feed carbon dioxides (S.18) are fed by two sections of synthesis reactor (5) lower parts, with two
Remaining reacting ethylene oxide in section synthesis reactor liquid phase feeding, two sections of obtained synthesis reactor liquid outlet streams
(S.15) it is flowed out by second stage reactor bottom, is sent out out-of-bounds after product pump surge tank (8) and by product pump (6) pressurization；
Iv it) is passed through by the total gaseous stream (S.14) obtained at the top of one section of synthesis reactor (1) and two sections of synthesis reactor (5)
It is discharged after the ethylene oxide that EO tourie (7) removing is wherein carried secretly.
It is emphasized that in the method, existing between different control points and influencing each other, such as when one section of synthetic reaction
When device temperature rise reduces, one section of synthesis reactor outer circulation control valve (V.1) aperture is reduced, and leads to one section of synthesis reactor extraction
Control valve (V.4) aperture increases, if obtaining without the adjustment effect of two sections of synthesis reactor extraction control valve (V.6)
Ethylene carbonate product purity will be unable to get control.
Preferably, one section of synthesis reactor liquid level is by one section of synthesis reactor extraction control valve (V.4) control.
Preferably, the circulating pump buffer tank pressure is controlled by circulating pump buffer tank pressure control valve (V.3).
Preferably, the circulating pump buffer tank pressure control valve can be controlled by surge tank liquid level signal or pressure signal.
It is highly preferred that the circulating pump buffer tank pressure control valve is controlled by buffer tank pressure signal.
Preferably, the synthesis reactor is one of fixed bed, bubbling bed and fluidized bed；It is highly preferred that the conjunction
It from bottom to top include liquid outlet opening, liquid hydraulic barrier, gas feed at reactor using phase reactor shown in attached drawing 3
Supporting screening plate under mouth, gas feed distributor, catalyst, catalyst layer, top porcelain layers of balls, props up on catalyst at lower part porcelain layers of balls
Support sieve plate, liquid inlet opening, liquid feed distributor and gas discharge mouth.
Preferably, the catalyst loaded in synthesis reactor is by weight, comprising:
A) component A:10-80 parts it is carried on SiO2Metal silicate on carrier, wherein metal silicate weight is group
The 1-50% of part A total weight；
B) alkyl silicate C has been grafted for component B:20-90 partsaHbXcSi(OR)3SiO2；Wherein a=3-23, b=7-
33, c=1-3, X N, P or S, R is-CH3Or-CH2CH3, alkyl silicate and SiO in grafting2Weight ratio be (0.002-
0.15): 1.
Preferably, synthesis reactor inlet temperature is 40-200 DEG C, and reaction pressure is normal pressure -10MPa；It is highly preferred that closing
It is 80-150 DEG C at reactor inlet temperature, reaction pressure 1.5-3MPa.
Preferably, the cooling temperature of recirculation cooler is 40-100 DEG C；It is highly preferred that the cooling temperature of recirculation cooler is
70-90℃。
Preferably, circulation logistics (S.11) accounts for the 50-99% of reactor liquid phase total feed；
It is highly preferred that circulation logistics (S.11) accounts for the 80-95% of reactor liquid phase total feed.
Wherein reactor liquid phase combined feed includes the merging logistics of circulation logistics (S.11) and ethylene oxide raw material (S.1).
Preferably, the ratio that one section of synthesis reactor feed carbon dioxide amount (S.4) accounts for carbon dioxide material quantity (S.2) is
1-99%.
It is highly preferred that one section of synthesis reactor feed carbon dioxide amount (S.4) accounts for the ratio of carbon dioxide material quantity (S.2)
For 40-90%.
Preferably, circulating pump buffer tank pressure is not higher than one section of synthesis reactor pressure, and product pump buffer tank pressure is not high
In two sections of synthesis reactor pressure.
It is highly preferred that circulating pump buffer tank pressure is 10KPa to normal pressure, product pump buffer tank pressure be normal pressure extremely
200KPa。
Preferably, one section of synthesis reactor outer circulation control valve (V.1) can be by one section of synthesis reactor catalyst bed
Any position temperature signal controls in temperature rise signal or catalyst bed.
It is highly preferred that one section of synthesis reactor outer circulation control valve (V.1) is by one section of synthesis reactor catalyst bed
Temperature rise signal control.
The present invention proposes a kind of control method of ethylene carbonate synthesis technology: (1) being controlled using outer circulation mass flow
Catalyst in reactor bed temperature rise processed guarantees bed temperature rise in a certain range；(2) go out oral fluid using one section of synthesis reactor
Phase produced quantity controls one section of synthesis reactor liquid level, controls product purity using second stage reactor outlet liquid phase produced quantity, guarantees
The complete conversion of ethylene oxide；(3) the gas phase regulating valve Staged cotrol pressure inside the tank and liquid level of circulating pump surge tank are utilized, it is ensured that
Gas can not enter external circulating system through circulating pump.The present invention achieves good technical effect.
Detailed description of the invention
Fig. 1 is the process flow diagram of the method for the present invention, and Fig. 2 is preferred ethylene carbonate synthesis reactor schematic diagram.
In Fig. 1,1 is one section of synthesis reactor, and 2 be product cooler, and 3 be circulating pump surge tank, and 4 be circulating pump, and 5 be two
Section synthesis reactor, 6 be product pump, and 7 be EO tourie, and 8 be product pump surge tank.
V.1 be one section of synthesis reactor outer circulation control valve, be V.2 one section of synthesis reactor pressure-control valve, V.3 for
V.4, circulating pump buffer tank pressure control valve produces control valve for one section of synthesis reactor, is V.5 two sections of synthesis reactor pressures
V.6, force control valve produces control valve for two sections of synthesis reactor.
S.1 it is ethylene oxide raw material, is S.2 carbon dioxide raw material, is S.3 ethylene oxide combined feed, be S.4 a Duan Hecheng
S.5, reactor feed carbon dioxide is one section of synthesis reactor gas vent logistics, is S.6 one section of synthesis reactor liquid discharge
S.7, mouth logistics, is product cooler outlet logistics, is S.8 that circulating pump buffers head space gas phase outlet streams, S.9 slow for circulating pump
Tank liquid phase exit stream is rushed, is S.10 circulating-pump outlet logistics, is S.12 two sections of synthesis reactor liquid phases S.11 to recycle logistics
S.13, charging, is two sections of synthesis reactor gas vent logistics, is S.14 total gaseous stream, be S.15 two sections of synthesis reactor liquid
S.16, body outlet streams are carbon dioxide gas effluent streams, are S.17 ethylene carbonate product, are S.18 two sections of synthetic reactions
S.19, device feed carbon dioxide is product pump surge tank and two sections of synthesis reactor balanced lines.
In Fig. 2,1 is liquid inlet opening, and 2 be gas feed mouth, and 3 be gas discharge mouth, and 4 be liquid outlet opening, and 5 be liquid
Import distributor, 6 be catalyst support sieve plate, and 7 be catalyst layer, and 8 be liquid hydraulic barrier, and 9 be porcelain layers of balls, 10 for gas into
Mouth distributor.
The present invention will be further described below by way of examples.
Specific embodiment
[embodiment 1]
Embodiment 1 is described below with reference to Fig. 1.
Process flow is as shown in Figure 1, ethylene oxide charging (S.1) flow is 100kg/h, into one section of synthesis reactor
(1) top, feed carbon dioxide (S.2) flow are 100kg/h, and therein 95% enters under one section of synthesis reactor (3)
Portion, reactor pressure control the liquid level in 2.5MPa, reactor by vapor delivery line pressure-control valve and go two sections of liquid phases to adopt by one section
Outflow control valve controls, and temperature rise is controlled by recycle stock flow control valve at about 20 DEG C in reactor.Reactor inlet temperature
It is 80 DEG C.When system reaches stable, liquid phase stream (S.6) temperature that one section of synthesis reactor bottom obtains is 100 DEG C or so, into
Enter circulating pump surge tank (3), liquid level is indirectly controlled by tank deck pressure-control valve 50% or so of tank height in surge tank, tank bottom
Liquid phase is cooled to 80 DEG C of rear portions (S.11 the 95% of logistics flux) through circulating pump (4) and recirculation cooler (2) and returns to reaction
Device entrance, remaining enters two sections of synthesis reactor (5) tops, remaining 5% two sections of synthesis reactor of entrance of feed carbon dioxide
Lower part.The inlet temperature of second stage reactor is 80 DEG C, operating pressure 2.5MPa.The liquid phase object obtained by second stage reactor bottom
Stream (S.15) amount is controlled by product purity, is sent out out-of-bounds through product pump surge tank (8) and product pump (6), product purity is
99.54%.
[comparative example 1]
1 process of comparative example is as shown in Figure 1, cancel two sections of synthesis reactor extraction control valve (V.6) in process.
Process flow is omitted herein as shown in Figure 1, technique and flow stream parameters are in the same manner as in Example 1.Due to operating
There is fluctuation in journey, therefore the purity of obtained ethylene carbonate product fluctuates between 90%-99.5%, leads to product quality
It is unable to get effective control.
[embodiment 2]
Embodiment 2 is described below with reference to Fig. 1.
Process flow is as shown in Figure 1, ethylene oxide charging (S.1) flow is 100kg/h, into one section of synthesis reactor
(1) top, feed carbon dioxide (S.2) flow are 100kg/h, and therein 80% enters under one section of synthesis reactor (3)
Portion, reactor pressure control the liquid level in 1.5MPa, reactor by vapor delivery line pressure-control valve and go two sections of liquid phases to adopt by one section
The control of outflow control valve, catalyst in reactor bed lower layer's temperature are controlled by recycle stock flow control valve at about 100 DEG C.
Reactor inlet temperature is 80 DEG C.When system reaches stable, liquid phase stream (S.6) temperature that one section of synthesis reactor bottom obtains
It is 100 DEG C or so, into circulating pump surge tank (3), liquid level is indirectly controlled by tank deck pressure-control valve in tank height in surge tank
30% or so, tank bottom liquid phase is cooled to 80 DEG C of rear portion (S.11 logistics fluxs through circulating pump (4) and recirculation cooler (2)
86%) Returning reactor entrance, remaining (S.12) enter two sections of synthesis reactor (5) tops, feed carbon dioxide remaining
20% enters two sections of synthesis reactor lower parts.The inlet temperature of second stage reactor is 80 DEG C, operating pressure 1.5MPa.By two sections
Liquid phase stream (S.15) amount that reactor bottom obtains is controlled by product purity, is sent through product pump surge tank (8) and product pump (6)
Outside out-of-bounds, product purity 99.05%.
[comparative example 2]
2 process of comparative example is as shown in Figure 1, one section of synthesis reactor outer circulation control valve (V.1) is changed to fix in process
Flow control.
Process flow is omitted herein as shown in Figure 1, technique and flow stream parameters are in the same manner as in Example 1.Due to operating
In journey there is fluctuation in the temperature rise of first stage reactor bed,, can not since outer circulation is firm discharge control when temperature rise increases by 10 DEG C
Temperature rise is adjusted, causes catalyst activity to reduce, product quality is equally made to be unable to get effective control.
[embodiment 3]
Embodiment 3 is described below with reference to Fig. 1.
Process flow is as shown in Figure 1, ethylene oxide charging (S.1) flow is 100kg/h, into one section of synthesis reactor
(1) top, feed carbon dioxide (S.2) flow are 100kg/h, and therein 70% enters under one section of synthesis reactor (3)
Portion, reactor pressure control the liquid level in 3.0MPa, reactor by vapor delivery line pressure-control valve and go two sections of liquid phases to adopt by one section
Outflow control valve controls, and temperature rise is controlled by recycle stock flow control valve at about 15 DEG C in reactor.Reactor inlet temperature
It is 90 DEG C.When system reaches stable, liquid phase stream (S.6) temperature that one section of synthesis reactor bottom obtains is 105 DEG C or so, into
Enter circulating pump surge tank (3), liquid level makes liquid level 40% or so of tank height by Liquid level in tank in surge tank, tank bottom liquid phase
90 DEG C of rear portions (S.11 the 90% of logistics flux) Returning reactor is cooled to through circulating pump (4) and recirculation cooler (2) to enter
Mouthful, remaining (S.12) enters two sections of synthesis reactor (5) tops, remaining 30% two sections of synthetic reaction of entrance of feed carbon dioxide
Device lower part.The inlet temperature of second stage reactor is 90 DEG C, operating pressure 3.0MPa.The liquid phase obtained by second stage reactor bottom
Logistics (S.15) amount is controlled by product purity, is sent out out-of-bounds through product pump surge tank (8) and product pump (6), product purity is
99.50%.
[comparative example 3]
3 process of comparative example is changed to fixed pressure as shown in Figure 1, cancel circulating pump buffer tank pressure control valve (V.3) in process
Power control.
Process flow is omitted herein as shown in Figure 1, technique and flow stream parameters are in the same manner as in Example 1.Due to operating
In journey there is fluctuation in first stage reactor pressure, when reactor pressure reduces, since circulating pump surge tank is fixation pressure control
And it is higher than reactor pressure, cause reaction product can not be from inflow circulating pump surge tank, and then outer circulation amount is caused to be interrupted, bed
Temperature runaway.
Control method in through the foregoing embodiment realizes following purpose: (1) using the temperature rise of first stage reactor bed come
It determines internal circulating load, prevents first stage reactor bed temperature rise is excessive from leading to temperature runaway；(2) it is adopted using one section of synthesis reactor outlet liquid phase
Output controls one section of synthesis reactor liquid level, controls product purity using second stage reactor outlet liquid phase produced quantity, makes epoxy second
Alkane converts completely, ensure that ethylene carbonate product purity；(3) the gas phase regulating valve Staged cotrol tank of circulating pump surge tank is utilized
Interior liquid level, it is ensured that gas can not enter external circulating system through circulating pump.
[embodiment 4]
Embodiment 4 is described below with reference to Fig. 1.
Process flow is as shown in Figure 1, ethylene oxide charging (S.1) flow is 100kg/h, into one section of synthesis reactor
(1) top, feed carbon dioxide (S.2) flow are 100kg/h, and therein 80% enters under one section of synthesis reactor (3)
Portion, reactor pressure control the liquid level in 1.5MPa, reactor by vapor delivery line pressure-control valve and go two sections of liquid phases to adopt by one section
The control of outflow control valve, catalyst in reactor bed lower layer's temperature are controlled by recycle stock flow control valve at about 100 DEG C.
Reactor inlet temperature is 80 DEG C.When system reaches stable, liquid phase stream (S.6) temperature that one section of synthesis reactor bottom obtains
It is 100 DEG C or so, into circulating pump surge tank (3), liquid level is indirectly controlled by tank deck pressure-control valve in tank height in surge tank
30% or so, tank bottom liquid phase is cooled to 80 DEG C of rear portion (S.11 logistics fluxs through circulating pump (4) and recirculation cooler (2)
86%) Returning reactor entrance, remaining (S.12) enter two sections of synthesis reactor (5) tops, feed carbon dioxide remaining
20% enters two sections of synthesis reactor lower parts.The inlet temperature of second stage reactor is 80 DEG C, operating pressure 1.5MPa.By two sections
Liquid phase stream (S.15) amount that reactor bottom obtains is controlled by product purity, is sent through product pump surge tank (8) and product pump (6)
Outside out-of-bounds, product purity 99.05%.
[comparative example 2]
2 process of comparative example is as shown in Figure 1, one section of synthesis reactor outer circulation control valve (V.1) control loop in process
Flow is react total feed 40%.
Process flow is omitted herein as shown in Figure 1, technique and flow stream parameters are in the same manner as in Example 1., due to outer circulation
It measures less than normal, is unable to control catalyst bed temperature rise, gradually rises bed temperature, catalyst activity is caused to reduce, make product matter
Amount is unable to get control.
Claims (9)
1. a kind of control method of ethylene carbonate synthesis technology, the synthesis of ethylene carbonate include one section of synthesis reactor (1),
Circulating pump surge tank (3), recirculation cooler (2), two sections of synthesis reactor (5), product pump surge tank (8), produces circulating pump (4)
Product pump (6) and EO tourie (7)；Ethylene oxide raw material (S.1) and carbon dioxide raw material (S.2) by one section of synthesis reactor and
After the reaction of two sections of synthesis reactor, ethylene carbonate product (S.17) is obtained；It is characterized in that one section of synthesis reactor catalysis
The temperature rise of agent bed is controlled by one section of synthesis reactor outer circulation control valve (V.1)；Ethylene carbonate product purity is closed by two sections
At reactor extraction control valve (V.6) control；
Wherein, the inlet temperature of synthesis reactor is 40-90 DEG C；
Circulation logistics (S.11) accounts for the 50-95% of reactor liquid phase total feed；And
The ratio that one section of synthesis reactor feed carbon dioxide amount (S.4) accounts for carbon dioxide material quantity (S.2) is 1-95%；
Wherein, ethylene carbonate synthesis technology the following steps are included:
I) ethylene oxide raw material (S.1) and one section of synthesis reactor feed carbon dioxide (S.4) respectively enter one section of synthetic reaction
The upper and lower part of device (1), and react in the reactor；
Ii the liquid outlet stream (S.6) and unreacted gas vent logistics that) reaction obtains in one section of synthesis reactor (1)
(S.5) it is flowed out respectively by the bottom and top of reactor；Liquid outlet stream enters circulating pump surge tank (3), isolated
The circulation that circulating pump surge tank liquid phase exit stream (S.9) obtains after circulating pump (4) are pressurized and recirculation cooler (2) is cooling
Logistics (S.11) is back to one section of synthesis reactor liquid phase entrance, remaining as two sections of synthesis reactor liquid phase feedings (S.12) into
Enter two sections of synthesis reactor (5) tops；
Iii) two sections of synthesis reactor feed carbon dioxides (S.18) are fed by two sections of synthesis reactor (5) lower parts, are closed with two sections
At remaining reacting ethylene oxide in reactor liquid phase feeding, obtained two sections of synthesis reactor liquid outlet streams (S.15) by
The outflow of second stage reactor bottom is sent out out-of-bounds after product pump surge tank (8) and by product pump (6) pressurization；
Iv it) is inhaled by the total gaseous stream (S.14) obtained at the top of one section of synthesis reactor (1) and two sections of synthesis reactor (5) through EO
It is discharged after the ethylene oxide that closed cans (7) removing is wherein carried secretly.
2. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that a Duan Hecheng
Reactor liquid level is by one section of synthesis reactor extraction control valve (V.4) control.
3. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that the circulating pump is slow
Pressure tank is rushed to be controlled by circulating pump buffer tank pressure control valve (V.3).
4. the control method of described in any item ethylene carbonate synthesis technologies according to claim 1~3, it is characterised in that described
Circulating pump buffer tank pressure control valve can be controlled by surge tank liquid level signal or pressure signal.
5. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that the synthetic reaction
Device is one of bubbling bed, fixed bed or fluidized bed.
6. the control method of ethylene carbonate synthesis technology according to claim 1-3, it is characterised in that synthesis
Reactor reaction pressure is normal pressure -10MPa.
7. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that recirculation cooler
Cooling temperature is 40-100 DEG C.
8. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that one section of synthetic reaction
The ratio that device feed carbon dioxide amount (S.4) accounts for carbon dioxide material quantity (S.2) is 40-90%.
9. the control method of ethylene carbonate synthesis technology according to claim 1, it is characterised in that one section of synthetic reaction
Device outer circulation control valve (V.1) can be by any in one section of synthesis reactor catalyst bed temperature rise signal or catalyst bed
The control of position temperature signal.
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| CN108484565B (en) * | 2018-03-30 | 2021-03-19 | 中国海洋石油集团有限公司 | System for producing carbonic ester and method for producing carbonic ester by using system |
| CN110028483A (en) * | 2019-04-30 | 2019-07-19 | 大连理工大学 | A kind of method that outer circulation atomizing gas-liquid contact technique prepares cyclic carbonate |
| CN110627764B (en) * | 2019-10-15 | 2020-08-25 | 西南化工研究设计院有限公司 | Ethylene carbonate production equipment system and production method thereof |
| CN112876450A (en) * | 2021-01-19 | 2021-06-01 | 中科院过程工程研究所南京绿色制造产业创新研究院 | Preparation method and application of cyclic carbonate |
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