CN109293512A - Esters of acrylic acid product production device - Google Patents

Esters of acrylic acid product production device Download PDF

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Publication number
CN109293512A
CN109293512A CN201811504241.4A CN201811504241A CN109293512A CN 109293512 A CN109293512 A CN 109293512A CN 201811504241 A CN201811504241 A CN 201811504241A CN 109293512 A CN109293512 A CN 109293512A
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China
Prior art keywords
gas
liquid
shell
tube reactor
liquid separator
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Pending
Application number
CN201811504241.4A
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Chinese (zh)
Inventor
秦振伟
秦敏锐
颜淑姬
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Qin Minrui
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Hangzhou Ruoshui Chemical Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Priority to CN201811504241.4A priority Critical patent/CN109293512A/en
Publication of CN109293512A publication Critical patent/CN109293512A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

This application discloses esters of acrylic acid product production device, including shell and tube reactor and injector, the injector connects with the feed inlet of shell and tube reactor, and the injector is used to for raw material to be injected into progress liquid film reaction in shell and tube reactor.The invention has the following beneficial effects: use shell and tube reactor, and reaction raw materials are the liquid filmization reactions carried out in shell and tube reactor, the usage amount for significantly reducing reaction solution reduces the yield of the three wastes in reaction process, and the phenomenon that be not in polymerization in reaction process.

Description

Esters of acrylic acid product production device
Technical field
The present invention relates to field of chemical equipment more particularly to a kind of esters of acrylic acid product production devices.
Background technique
Acrylate, methyl acrylic ester product are a kind of polymer monomers haveing excellent performance, and general synthetic method is Acrylic acid (methacrylic acid), which reacts under acidic catalyst effect with alcohol or hydroxyl, generates ester.Production this kind of product uses at present Acryloyl chloride (methacrylic chloride) is reacted with alcohol or hydroxyl does not need higher temperature, but reacts generally in nonaqueous solvents Middle progress, equipment used are common reaction kettle, need to be added a large amount of alkali into reaction kettle (with solution in reaction process Form heaven) it is used as acid binding agent, due to needing to use a large amount of solution, so the more three wastes can be generated, simultaneously because It carries out in a kettle, will appear polymerism during the reaction.
Summary of the invention
The present invention is in view of the above-mentioned problems, propose a kind of esters of acrylic acid product production device.
The technical solution adopted by the present invention is as follows:
A kind of esters of acrylic acid product production device, including shell and tube reactor and injector, the injector and tubulation The feed inlet of formula reactor connects, and the injector is used to for raw material to be injected into progress liquid film reaction in shell and tube reactor.
It should be noted that the shell and tube reactor of the present apparatus belongs to existing apparatus, setting in the tubulation of shell and tube reactor There is filler, when reaction raw materials (liquid) are after injector spirt shell and tube reactor, liquid passes through in shell and tube reactor Distribution grid enters tubulation, forms liquid film in tubulation wall and filler surface, is reacted by way of liquid film, the reaction of liquid film Form can reduce the usage amount of solution, greatly reduce the yield of the three wastes, while during the reaction be not in polymerization Phenomenon.
The present apparatus due to use shell and tube reactor, and reaction raw materials shell and tube reactor be carry out liquid filmization it is anti- It answers, significantly reduces the usage amount of reaction solution, reduce the yield of the three wastes in reaction process, and will not go out in reaction process The phenomenon that now polymerizeing.
It optionally, further include the first gas-liquid separator, the feed end and shell and tube reactor of first gas-liquid separator Top exit connect, the outlet side of the first gas-liquid separator connects with raw material recovery device, the first gas-liquid separator go out liquid End connects with the liquid return hole of shell and tube reactor.
Shell and tube reactor is in a vertical state when in use, and the top exit of shell and tube reactor is located at the upper of reactor At end.What is left from top exit is the mixture of pure and mild ester, and the mixture of the two enters the first gas-liquid point as a vapor From device, low-boiling alcohol (gaseous state) enters raw material recovery device, and high boiling ester (liquid condition) continues traveling downwardly leads to again It crosses liquid return hole and enters in shell and tube reactor that the reaction was continued.
Optionally, raw material recovery device include the first condenser and recycling storage tank, the outlet end of first condenser with Recycling storage tank connects, and the input end of first condenser connects with the first gas-liquid separator.
Low-boiling alcohol by gaseous state is transformed into liquid condition after the processing of the first condenser, then liquid alcohol into Enter to recycle storage tank and further recycle.
It optionally, further include the second gas-liquid separator, the feed end and shell and tube reactor of second gas-liquid separator Outlet at bottom connect, the outlet end of the second gas-liquid separator connects with product collecting device, second gas-liquid separator Outlet side connects with the input end of the first condenser.
The liquid-type left from outlet at bottom contains the liquid of product, in this partially liq still containing it is more can be again The alcohol utilized, so the second gas-liquid separator of setting, so as to enter the first condenser in gaseous form further for this part alcohol Condensation utilizes.
Optionally, the product collecting device includes collecting tank and the second condenser, the input end of second condenser Connect with the outlet end of the second gas-liquid separator, the outlet end of the second condenser connects with collecting tank.
Because still temperature is higher from the liquid (product is located in this partially liq) that the second gas-liquid separator flows out, So further being utilized after reducing the temperature of this partially liq using the second condenser.
It optionally, further include diaphragm pump, second gas-liquid separator passes through the bottom of diaphragm pump and shell and tube reactor Outlet connects, and the diaphragm pump is for the liquid flowed out in shell and tube reactor to be delivered in the second gas-liquid separator.
Optionally, further include sprayer, the sprayer is provided between the diaphragm pump and the second gas-liquid separator, and The sprayer is set on the feed end of the second gas-liquid separator, and the liquid that sprayer is used to come diaphragm pump conveying is with liquid The form of mist is injected into the second gas-liquid separator.
Optionally, the injector is venturi-type eductors.
Optionally, further include gas tank and heat exchanger, described heat exchanger one end connects with gas tank, heat exchanger it is another End connects with the gas feed of tubular heat exchanger;Inert gas is stored in the gas tank, the heat exchanger is for being fed Enter the inert gas heating of shell and tube reactor.
Inert gas used in this programme preferentially uses nitrogen, and the purpose in the present apparatus with nitrogen is in order to will to be located at The material of shell and tube reactor bottom blows to top and is reacted, and whole process is similar to the reaction in ebullated bed.
It is reacted it should be noted that the present apparatus is used in using acrylic acid (methacrylic acid) with alcohol or hydroxyl to prepare Acrylate, methyl acrylic ester product, while also using the present apparatus when the such product of ester-interchange method.
The beneficial effects of the present invention are: using shell and tube reactor, and reaction raw materials are to carry out in shell and tube reactor Liquid filmization reaction, significantly reduce the usage amount of reaction solution, reduce the yield of the three wastes in reaction process, and reacted The phenomenon that being not in polymerization in journey.
Detailed description of the invention:
Fig. 1 is esters of acrylic acid product production device schematic diagram.
Each appended drawing reference in figure are as follows: 1, reactor, 101, top exit, 102, liquid return hole, 103, outlet at bottom, 2, Wen Qiu In injector, the 301, first gas-liquid separator, the 302, second gas-liquid separator, the 401, first condenser, the 402, second condenser, 5, recycling storage tank, 6, collecting tank, 7, diaphragm pump, 8, sprayer, 9, gas tank, 10, heat exchanger, 11, pressure reducing valve, 12, flowmeter, 13, raw material mixing kettle, 14, delivery pump.
Specific embodiment:
Below with reference to each attached drawing, the present invention will be described in detail.
A kind of esters of acrylic acid product production device, including shell and tube reactor 1 and injector, the injector and tubulation The feed inlet of formula reactor 1 connects, and it is anti-that the injector is used to for raw material being injected into progress liquid filmization in shell and tube reactor 1 It answers.
It should be noted that the shell and tube reactor 1 of the present apparatus belongs to existing apparatus, set in the tubulation of shell and tube reactor 1 It is equipped with filler, when reaction raw materials (liquid) are after injector spirt shell and tube reactor 1, liquid passes through shell and tube reactor 1 Interior distribution grid enters tubulation, forms liquid film in tubulation wall and filler surface, is reacted by way of liquid film, liquid film Reaction formation can reduce the usage amount of solution, greatly reduce the yield of the three wastes, while being not in during the reaction Polymerism.
The present apparatus is due to using shell and tube reactor 1, and reaction raw materials are the liquid films carried out in shell and tube reactor 1 Reaction, significantly reduces the usage amount of reaction solution, reduces the yield of the three wastes in reaction process, and will not in reaction process The phenomenon that polymerizeing.
It as shown in Fig. 1, further include the first gas-liquid separator 301, the feed end and column of first gas-liquid separator 301 The top exit 101 of tubular reactor 1 connects, and the outlet side of the first gas-liquid separator 301 connects with raw material recovery device, and first The outlet end of gas-liquid separator 301 connects with the liquid return hole 102 of shell and tube reactor 1.
Shell and tube reactor 1 is in a vertical state when in use, and the top exit 101 of shell and tube reactor 1 is located at reaction At the upper end of device 1.What is left from top exit 101 is the mixture of pure and mild ester, and the mixture of the two enters as a vapor First gas-liquid separator 301, low-boiling alcohol (gaseous state) enter raw material recovery device, high boiling ester (liquid condition) after Continuous downlink is again through the reaction was continued in the entrance shell and tube reactor 1 of liquid return hole 102.
As shown in Fig. 1, raw material recovery device includes the first condenser 401 and recycling storage tank 5, first condenser 401 outlet end connects with recycling storage tank 5, and the input end of first condenser 401 connects with the first gas-liquid separator 301.
Low-boiling alcohol is transformed into liquid condition by gaseous state after the processing of the first condenser 401, then liquid Alcohol enters recycling storage tank 5 and further recycles.
It as shown in Fig. 1, further include the second gas-liquid separator 302, the feed end and column of second gas-liquid separator 302 The outlet at bottom 103 of tubular reactor 1 connects, and the outlet end of the second gas-liquid separator 302 connects with product collecting device, described The outlet side of second gas-liquid separator 302 connects with the input end of the first condenser 401.
The liquid-type left from outlet at bottom 103 contains the liquid of product, in this partially liq still containing it is more can be with The alcohol utilized again, so the second gas-liquid separator 302 of setting, so that this part alcohol enters the first condenser in gaseous form 401 further condensation utilizations.
As shown in Fig. 1, the product collecting device includes collecting tank 6 and the second condenser 402, second condenser 402 input end connects with the outlet end of the second gas-liquid separator 302, outlet end and 6 phase of collecting tank of the second condenser 402 It connects.
Because of the liquid (product is located in this partially liq) flowed out from the second gas-liquid separator 302, still temperature compared with Height, so using further being utilized after temperature of second condenser 402 to reduce this partially liq.
It as shown in Fig. 1, further include diaphragm pump 7, second gas-liquid separator 302 is anti-by diaphragm pump 7 and shell and tube The outlet at bottom 103 of device 1 is answered to connect, the diaphragm pump 7 is used to the liquid flowed out in shell and tube reactor 1 being delivered to the second gas In liquid/gas separator 302.
As shown in Fig. 1, further include sprayer 8, be arranged between the diaphragm pump 7 and the second gas-liquid separator 302 Sprayer 8 is stated, and the sprayer 8 is set on the feed end of the second gas-liquid separator 302, sprayer 8 is used for diaphragm pump 7 The liquid to come is conveyed to be injected into the form of liquid mist in the second gas-liquid separator 302.
As shown in Fig. 1, the injector is venturi-type eductors 2.
It as shown in Fig. 1, further include gas tank 9 and heat exchanger 10, described 10 one end of heat exchanger connects with gas tank 9, heat The other end of exchanger 10 connects with the gas feed of tubular heat exchanger;Inert gas, the heat are stored in the gas tank 9 Exchanger 10 is used to be fed to heat into the inert gas of shell and tube reactor 1.
Inert gas used in this programme preferentially uses nitrogen, and the purpose in the present apparatus with nitrogen is in order to will to be located at The material of 1 bottom of shell and tube reactor blows to top and is reacted, and whole process is similar to the reaction in ebullated bed.
It is reacted it should be noted that the present apparatus is used in using acrylic acid (methacrylic acid) with alcohol or hydroxyl to prepare Acrylate, methyl acrylic ester product, while also using the present apparatus when the such product of ester-interchange method.
As shown in Fig. 1, reaction raw materials are mixed in raw material mixing kettle 13, are mixed and are completed in raw material mixing kettle 13 Afterwards, then by delivery pump 14 venturi-type eductors 2 are delivered to.
As shown in Fig. 1, it in order to monitor the gas outflow in gas tank, is provided between gas tank 9 and heat exchanger 10 Pressure reducing valve 11 and flowmeter 12.
The above description is only a preferred embodiment of the present invention, not thereby limits scope of patent protection of the invention, all It is directly or indirectly to be used in other relevant technologies with equivalent structure transformation made by description of the invention and accompanying drawing content Field similarly includes within the scope of the present invention.

Claims (9)

1. a kind of esters of acrylic acid product production device, which is characterized in that including shell and tube reactor and injector, the injection Device connects with the feed inlet of shell and tube reactor, and the injector carries out liquid film for raw material to be injected into shell and tube reactor Change reaction.
2. esters of acrylic acid product production device as described in claim 1, which is characterized in that further include the first gas-liquid separation The feed end of device, first gas-liquid separator connects with the top exit of shell and tube reactor, and the first gas-liquid separator goes out Gas end connects with raw material recovery device, and the outlet end of the first gas-liquid separator connects with the liquid return hole of shell and tube reactor.
3. esters of acrylic acid product production device as claimed in claim 2, which is characterized in that raw material recovery device includes first The outlet end of condenser and recycling storage tank, first condenser connects with recycling storage tank, the input end of first condenser Connect with the first gas-liquid separator.
4. esters of acrylic acid product production device as claimed in claim 3, which is characterized in that further include the second gas-liquid separation The feed end of device, second gas-liquid separator connects with the outlet at bottom of shell and tube reactor, and the second gas-liquid separator goes out Liquid end connects with product collecting device, and the outlet side of second gas-liquid separator connects with the input end of the first condenser.
5. esters of acrylic acid product production device as claimed in claim 4, which is characterized in that the product collecting device includes The input end of collecting tank and the second condenser, second condenser connects with the outlet end of the second gas-liquid separator, and second is cold The outlet end of condenser connects with collecting tank.
6. esters of acrylic acid product production device as claimed in claim 4, which is characterized in that it further include diaphragm pump, described Two gas-liquid separators are connected by diaphragm pump with the outlet at bottom of shell and tube reactor, and the diaphragm pump is used for tubular reaction The liquid flowed out in device is delivered in the second gas-liquid separator.
7. esters of acrylic acid product production device as claimed in claim 6, which is characterized in that further include sprayer, it is described every Be provided with the sprayer between membrane pump and the second gas-liquid separator, and the sprayer be set to the second gas-liquid separator into Expect on end, sprayer is used to for the liquid that diaphragm pump conveying comes being injected into the form of liquid mist in the second gas-liquid separator.
8. esters of acrylic acid product production device as described in claim 1, which is characterized in that the injector is venturi spray Emitter.
9. esters of acrylic acid product production device as described in claim 1, which is characterized in that further include gas tank and heat exchange Device, described heat exchanger one end connect with gas tank, and the other end of heat exchanger connects with the gas feed of tubular heat exchanger;Institute It states and stores inert gas in gas tank, the heat exchanger is used to be fed to heat into the inert gas of shell and tube reactor.
CN201811504241.4A 2018-12-10 2018-12-10 Esters of acrylic acid product production device Pending CN109293512A (en)

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CN201811504241.4A CN109293512A (en) 2018-12-10 2018-12-10 Esters of acrylic acid product production device

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Application Number Priority Date Filing Date Title
CN201811504241.4A CN109293512A (en) 2018-12-10 2018-12-10 Esters of acrylic acid product production device

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110511142A (en) * 2019-08-29 2019-11-29 青岛科技大学 A kind of continuous production system and production technology of methylvinyl acetate
CN115894172A (en) * 2022-10-14 2023-04-04 青岛科技大学 Continuous production system and method of 2, 5-dimethyl-2, 5-hexanediol

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CN105254583A (en) * 2015-11-20 2016-01-20 河北德瑞化工有限公司 Method for preparing 2-chloro-5-chloromethylthiazole by jet loop reactor
CN108311088A (en) * 2017-01-17 2018-07-24 浙江大学 Injecting type annular-pipe reactor and the method for preparing butyl type rubber polymer
CN209759344U (en) * 2018-12-10 2019-12-10 杭州若水化学科技有限公司 Acrylic ester product production device
CN111971266A (en) * 2018-03-28 2020-11-20 三菱化学株式会社 Method for producing unsaturated carboxylic acid ester

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* Cited by examiner, † Cited by third party
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JPH0352842A (en) * 1989-07-21 1991-03-07 Nippon Shokubai Kagaku Kogyo Co Ltd Production of methacrylic acid ester
JPH08143512A (en) * 1994-11-25 1996-06-04 Lucky Ltd Process and apparatus for producing unsaturated carboxylic acid ester
US5866713A (en) * 1996-08-20 1999-02-02 Mitsubishi Chemical Corporation Method for preparing (meth)acrylic acid ester
US5785933A (en) * 1997-01-21 1998-07-28 Mobil Oil Corporation Sulfuric acid alkylation reactor system with static mixers
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CN204294235U (en) * 2014-11-28 2015-04-29 江门谦信化工发展有限公司 A kind of reactor device producing butyl acrylate with intubate
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110511142A (en) * 2019-08-29 2019-11-29 青岛科技大学 A kind of continuous production system and production technology of methylvinyl acetate
CN115894172A (en) * 2022-10-14 2023-04-04 青岛科技大学 Continuous production system and method of 2, 5-dimethyl-2, 5-hexanediol

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