CN110511142A - A kind of continuous production system and production technology of methylvinyl acetate - Google Patents

A kind of continuous production system and production technology of methylvinyl acetate Download PDF

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Publication number
CN110511142A
CN110511142A CN201910806778.4A CN201910806778A CN110511142A CN 110511142 A CN110511142 A CN 110511142A CN 201910806778 A CN201910806778 A CN 201910806778A CN 110511142 A CN110511142 A CN 110511142A
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CN
China
Prior art keywords
methylvinyl acetate
storage tank
venturi
reaction kettle
acetone
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CN201910806778.4A
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Chinese (zh)
Inventor
段振亚
董晓赛
张俊梅
王磊
李文辰
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Priority to CN201910806778.4A priority Critical patent/CN110511142A/en
Publication of CN110511142A publication Critical patent/CN110511142A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C07C67/46—Preparation of carboxylic acid esters from ketenes or polyketenes

Abstract

The invention discloses a kind of continuous production system of methylvinyl acetate and production technologies, including ketenes storage tank, catalyst storage tank, acetone storage tank, stirred tank, reaction kettle, heat exchanger and product storage tank, the catalyst storage tank and acetone storage tank are separately connected stirred tank feeding inlet；Venturi-type eductors, the stirred tank outlet connection venturi-type eductors liquid phase entrance are equipped at the top of the reaction kettle, the ketenes outlet connects venturi-type eductors gas phase entrance, and the reaction kettle outlet is sequentially connected heat exchanger and product storage tank.Production system of the invention, can be continuously produced methylvinyl acetate, can effectively save energy consumption and cost, and produce methylvinyl acetate product purity up to 72%.

Description

A kind of continuous production system and production technology of methylvinyl acetate
Technical field
The present invention relates to chemical technology fields, and in particular to a kind of continuous production system of methylvinyl acetate and production Technique.
Background technique
Methylvinyl acetate is slightly soluble in water, miscible in ethyl alcohol, ether and nonvolatile oil.In medicine, isopropyl acetate alkene Ester can be used as refining solvent or electron level solvent of fluocinolone acetonide series of products etc., can also make extraction solvent.In industry, isopropyl acetate Enester is widely used, such as can be used as the intermediate raw material of synthesis acetylacetone,2,4-pentanedione.Therefore, a kind of efficient methylvinyl acetate Production technology is economic value with higher.
In the production technology of existing methylvinyl acetate: the patent of Publication No. CN105777511A, acetone, catalyst are mixed Closing liquid and ketene gas hybrid mode are as follows: acetone, catalyst mixed liquid are directly added into the reaction kettle full of ketene gas, Then 300 DEG C -400 DEG C are heated up to；The defect of the technique is acetone, catalyst mixed liquid undercompounding, and acetone, catalysis Agent mixed liquor and ketenes contact area are small, and reaction efficiency is low, and energy consumption is high.The patent of Publication No. CN105777540A, acetone, Catalyst mixed liquid, which is evaporated into gas and is passed through in reaction kettle together with ketene gas, is reacted, and methylvinyl acetate is generated Crude product, crude product are refined again, and acetone and catalyst are evaporated into gas in the production technology, are consumed energy higher, and isopropyl acetate alkene Ester forms crude product, then is refined, this needs is carried out in two steps, comparatively laborious.
Summary of the invention
It is an object of the invention to overcome disadvantage of the existing technology, a kind of continuous metaplasia of methylvinyl acetate is provided Production system and production technology.
To achieve the goals above, a technical solution of the invention is: a kind of continuous production of methylvinyl acetate System, it is characterised in that: including ketenes storage tank, catalyst storage tank, acetone storage tank, stirred tank, reaction kettle, heat exchanger and product Storage tank,
Catalyst feeding inlet and acetone feeding inlet are equipped at the top of the stirred tank, the catalyst outlet passes through pipeline successively Connection flow control valve A and stirred tank catalyst feeding inlet, the acetone outlet are sequentially connected flow control by pipeline Valve B and stirred tank acetone feeding inlet；
Venturi-type eductors are equipped at the top of the reaction kettle, the stirred tank outlet is sequentially connected pump A, flow control by pipeline Valve D and venturi-type eductors liquid phase entrance, the ketenes outlet are sequentially connected flow control valve C and Wen Qiu by pipeline In injector gas phase entrance, reaction kettle outlet is sequentially connected pump B, heat exchanger, flow control valve E and product storage by pipeline Tank.
Further；Exhaust outlet is additionally provided at the top of the reaction kettle, the exhaust outlet connects gas exhaust piping, the exhaust pipe Road merges with ketenes outlet pipeline, and the gas exhaust piping is equipped with check valve.
Further；The stirred tank outer wall and reaction kettle outer wall are equipped with heating jacket.
Further；The pump A is mechanical pump, and pump B is metering pump.
Further；It is divided into two branches after the heat exchanger exit connecting line, the first branch connects venturi injection Device liquid phase entrance, second branch are sequentially connected flow control valve E and product storage tank.
A technical solution of the invention is: a kind of continuous producing method of methylvinyl acetate, which is characterized in that including Following steps:
(1) 50:1 enters stirred tank by volume for acetone and catalyst, is heated to 40 DEG C, through mechanical pump and flow after being uniformly mixed Control valve D enters venturi-type eductors liquid phase entrance；
(2) acetone and catalyst form high-speed jet inside venturi-type eductors, and negative pressure is formed inside venturi-type eductors Area, ketene gas are inhaled into venturi-type eductors, are sprayed into reaction kettle after mixing with acetone and catalyst with spray pattern It is reacted, generates methylvinyl acetate crude product；
(3) methylvinyl acetate crude product enters heat exchanger through metering pump, after cooling, returns to venturi-type eductors liquid phase entrance Into reaction kettle, after multi-reflow, turn-on flow rate control valve E makes methylvinyl acetate product a part enter product storage tank, Another part continues reflux purification；Unreacted ketene gas uplink is followed after the discharge of reaction kettle top vent in reaction kettle Ring utilizes.
Further；The catalyst is acetylsulfonic acid.
Further；The molar ratio of the acetone and ketenes is 1:1.
Further；Reaction temperature described in step (2) is 60 DEG C -70 DEG C.
Further；When methylvinyl acetate product purity in heat exchanger described in step (3) >=65%, turn-on flow rate control Valve E processed, control first branch bypass flow and second branch bypass flow ratio are 50:1, make methylvinyl acetate product one Divide and enter product storage tank, another part continues reflux purification.
Beneficial effects of the present invention:
(1) production system of the invention, can be continuously produced methylvinyl acetate, can effectively save energy consumption and cost, and produce Methylvinyl acetate product purity up to 72%.
(2) acetone, catalyst liquid and ketene gas are sprayed into reaction kettle by venturi-type eductors with spray pattern It is reacted, atomization reaction raw materials can increase heating surface area and contact surface area, to increase reaction efficiency, it is pure to improve product Degree.
Detailed description of the invention
Fig. 1 is production system schematic diagram of the present invention.
In figure: 1, ketenes storage tank；2, acetylsulfonic acid storage tank；3, acetone storage tank；4, stirred tank；41, steam heating jacket A；5, reaction kettle；51, steam heating jacket B；6, heat exchanger；7, product storage tank；8, venturi-type eductors；11, flow control valve A；12, flow control valve B；13, flow control valve C；14, flow control valve D；15, flow control valve E；16, mechanical pump；17, it counts Amount pump；18, check valve；L1, the first branch；L2, second branch；L3, gas exhaust piping.
Specific embodiment
Embodiment 1:
A kind of continuous production system of methylvinyl acetate, including ketenes storage tank 1, acetylsulfonic acid storage tank 2, acetone storage tank 3, Stirred tank 4, reaction kettle 5, heat exchanger 6 and product storage tank 7；Acetylsulfonic acid feeding inlet is equipped at the top of the stirred tank 4 and acetone enters Material mouth, the outlet of acetylsulfonic acid storage tank 2 are sequentially connected 4 acetylsulfonic acid pan feeding of flow control valve A11 and stirred tank by pipeline Mouthful, the outlet of acetone storage tank 3 is sequentially connected 4 acetone feeding inlet of flow control valve B12 and stirred tank by pipeline；The reaction It is equipped with feeding inlet at the top of kettle 5, venturi-type eductors 8 are equipped in the feeding inlet, the outlet of stirred tank 4 is successively connected by pipeline Connect 8 liquid phase entrance of mechanical pump 16, flow control valve D14 and venturi-type eductors, the outlet of ketenes storage tank 1 by pipeline according to 8 gas phase entrance of secondary connection flow control valve C13 and venturi-type eductors, the outlet of reaction kettle 5 are sequentially connected meter by pipeline Amount pumps 17 and heat exchanger 6, and two branches, the spray of first branch L1 connection venturi are divided into behind the 6 outlet connecting pipe road of heat exchanger 8 liquid phase entrance of emitter, second branch L2 are sequentially connected flow control valve E15 and product storage tank 7.
Be additionally provided with exhaust outlet at the top of the reaction kettle 5, the exhaust outlet connects gas exhaust piping L3, the gas exhaust piping L3 with 1 export pipeline of ketenes storage tank merges, and the gas exhaust piping L3 is equipped with check valve 18, and the check valve 18 is flowed to towards ketenes 1 export pipeline of storage tank.
4 outer wall of stirred tank is equipped with steam heating jacket A41, and 5 outer wall of reaction kettle is equipped with steam heating jacket B51。
Embodiment 2:
A kind of continuous production processes of methylvinyl acetate, which comprises the following steps:
(1) 50:1 enters stirred tank 4 by volume for acetone and acetylsulfonic acid, adds to 20L, is heated to 40 DEG C, passes through after stirring evenly Mechanical pump 16 and flow control valve D14 enter 8 liquid phase entrance of venturi-type eductors with the volume flow of 2.2mL/s；
(2) acetone and acetylsulfonic acid form high-speed jet inside venturi-type eductors 8, are formed inside venturi-type eductors 8 Negative pressuren zone, negative pressure 0.096MPa, ketene gas are inhaled into venturi-type eductors 8, after mixing with acetone and acetylsulfonic acid It is sprayed into reaction kettle 5 and is reacted with spray pattern, reaction temperature is 60 DEG C, generates methylvinyl acetate crude product, the acetone Molar ratio with ketenes is 1:1；
(3) methylvinyl acetate crude product enters heat exchanger 6 through metering pump 17, after being cooled to 55 DEG C, returns to 8 liquid of venturi-type eductors Phase entrance enters reaction kettle 5, refines through multi-reflow, when methylvinyl acetate product purity in heat exchanger 6 >=65%, opens stream Control valve E15, controls first branch L1 bypass flow in conjunction with metering pump 17 and second branch L2 bypass flow ratio is 50:1, Methylvinyl acetate product a part is set to enter product storage tank 7, another part continues reflux purification；When reflux, isopropyl acetate alkene Ester crude product forms negative pressure in venturi-type eductors 8, and unreacted ketene gas in reaction kettle 5 is inhaled by gas exhaust piping L3 Into venturi-type eductors 8, reacted with being sprayed into reaction kettle 5 after the mixing of unreacted acetone with spray pattern.Final products The purity of methylvinyl acetate product is 72% in storage tank 7.
Embodiment 3:
A kind of continuous production processes of methylvinyl acetate, which comprises the following steps:
(1) 50:1 enters stirred tank 4 by volume for acetone and acetylsulfonic acid, adds to 40L, is heated to 40 DEG C, passes through after stirring evenly Mechanical pump 16 and flow control valve D14 enter 8 liquid phase entrance of venturi-type eductors with the volume flow of 2.2mL/s；
(2) acetone and acetylsulfonic acid form high-speed jet inside venturi-type eductors 8, are formed inside venturi-type eductors 8 Negative pressuren zone, negative pressure 0.096MPa, ketene gas are inhaled into venturi-type eductors 8, after mixing with acetone and acetylsulfonic acid It is sprayed into reaction kettle 5 and is reacted with spray pattern, reaction temperature is 70 DEG C, generates methylvinyl acetate crude product, the acetone Molar ratio with ketenes is 1:1；
(3) methylvinyl acetate crude product enters heat exchanger 6 through metering pump 17, after being cooled to 55 DEG C, returns to 8 liquid of venturi-type eductors Phase entrance enters reaction kettle 5, refines through multi-reflow, when methylvinyl acetate product purity in heat exchanger 6 >=65%, opens stream Control valve E15, controls first branch L1 bypass flow in conjunction with metering pump 17 and second branch L2 bypass flow ratio is 50:1, Methylvinyl acetate product a part is set to enter product storage tank 7, another part continues reflux purification；When reflux, isopropyl acetate alkene Ester crude product forms negative pressure in venturi-type eductors 8, and unreacted ketene gas in reaction kettle 5 is inhaled by gas exhaust piping L3 Into venturi-type eductors 8, reacted with being sprayed into reaction kettle 5 after the mixing of unreacted acetone with spray pattern.Final products The purity of methylvinyl acetate product is 72% in storage tank 7.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of continuous production system of methylvinyl acetate, it is characterised in that: including ketenes storage tank, catalyst storage tank, Acetone storage tank, stirred tank, reaction kettle, heat exchanger and product storage tank,
Catalyst feeding inlet and acetone feeding inlet are equipped at the top of the stirred tank, the catalyst outlet passes through pipeline successively Connection flow control valve A and stirred tank catalyst feeding inlet, the acetone outlet are sequentially connected flow control by pipeline Valve B and stirred tank acetone feeding inlet；
Venturi-type eductors are equipped at the top of the reaction kettle, the stirred tank outlet is sequentially connected pump A, flow control by pipeline Valve D and venturi-type eductors liquid phase entrance, the ketenes outlet are sequentially connected flow control valve C and Wen Qiu by pipeline In injector gas phase entrance, reaction kettle outlet is sequentially connected pump B, heat exchanger, flow control valve E and product storage by pipeline Tank.
2. the continuous production system of methylvinyl acetate according to claim 1, it is characterised in that: the reaction kettle top Portion is additionally provided with exhaust outlet, and the exhaust outlet connects gas exhaust piping, and the gas exhaust piping merges with ketenes outlet pipeline, institute Gas exhaust piping is stated equipped with check valve.
3. the continuous production system of methylvinyl acetate according to claim 1, it is characterised in that: outside the stirred tank Wall and reaction kettle outer wall are equipped with heating jacket.
4. the continuous production system of methylvinyl acetate according to claim 1, it is characterised in that: the pump A is machine Tool pump, pump B are metering pump.
5. the continuous production system of methylvinyl acetate according to claim 1, it is characterised in that: the heat exchanger goes out It is divided into two branches after mouth connecting line, the first branch connects venturi-type eductors liquid phase entrance, and second branch is sequentially connected stream Control valve E and product storage tank.
6. a kind of method using the continuous production system production methylvinyl acetate described in claim 5, which is characterized in that The following steps are included:
(1) 50:1 enters stirred tank by volume for acetone and catalyst, is heated to 40 DEG C, through mechanical pump and flow after being uniformly mixed Control valve D enters venturi-type eductors liquid phase entrance；
(2) acetone and catalyst form high-speed jet inside venturi-type eductors, and negative pressure is formed inside venturi-type eductors Area, ketene gas are inhaled into venturi-type eductors, are sprayed into reaction kettle after mixing with acetone and catalyst with spray pattern It is reacted, generates methylvinyl acetate crude product；
(3) methylvinyl acetate crude product enters heat exchanger through metering pump, after cooling, returns to venturi-type eductors liquid phase entrance Into reaction kettle, after multi-reflow, turn-on flow rate control valve E makes methylvinyl acetate product a part enter product storage tank, Another part continues reflux purification；Unreacted ketene gas uplink is followed after the discharge of reaction kettle top vent in reaction kettle Ring utilizes.
7. the method for production methylvinyl acetate according to claim 6, it is characterised in that: the catalyst is acetyl sulphur Acid.
8. the method for production methylvinyl acetate according to claim 6, it is characterised in that: the acetone and ketenes Molar ratio is 1:1.
9. the method for production methylvinyl acetate according to claim 6, it is characterised in that: reacted described in step (2) Temperature is 60 DEG C -70 DEG C.
10. the method for production methylvinyl acetate according to claim 6, it is characterised in that: heat exchanger described in step (3) When interior methylvinyl acetate product purity >=65%, turn-on flow rate control valve E, control first branch bypass flow and second branch point Stream flow ratio is 50:1, and methylvinyl acetate product a part is made to enter product storage tank, and another part continues reflux purification.
CN201910806778.4A 2019-08-29 2019-08-29 A kind of continuous production system and production technology of methylvinyl acetate Pending CN110511142A (en)

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