CN106824017A - Auxiliary reactor for producing methyl butynol - Google Patents

Auxiliary reactor for producing methyl butynol Download PDF

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Publication number
CN106824017A
CN106824017A CN201710149765.5A CN201710149765A CN106824017A CN 106824017 A CN106824017 A CN 106824017A CN 201710149765 A CN201710149765 A CN 201710149765A CN 106824017 A CN106824017 A CN 106824017A
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CN
China
Prior art keywords
auxiliary reactor
hole plate
methyl butynol
communicated
reaction
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
CN201710149765.5A
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Chinese (zh)
Inventor
郭强
石茂平
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Luzhou Sichuan Ju Hong Chemical Industry LLC
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Luzhou Sichuan Ju Hong Chemical Industry LLC
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Application filed by Luzhou Sichuan Ju Hong Chemical Industry LLC filed Critical Luzhou Sichuan Ju Hong Chemical Industry LLC
Priority to CN201710149765.5A priority Critical patent/CN106824017A/en
Publication of CN106824017A publication Critical patent/CN106824017A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/44Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by addition reactions, i.e. reactions involving at least one carbon-to-carbon double or triple bond

Abstract

The present invention relates to a kind of production equipment of methyl butynol, a kind of auxiliary reactor for producing methyl butynol, including auxiliary reactor main body are specifically disclosed, be communicated in the overflow pipe of auxiliary reactor lower body part, be communicated in the discharge nozzle of auxiliary reactor body top;Auxiliary reactor lower body part is provided with hole plate, and overflow pipe is communicated on the wall below hole plate.It is an advantage of the invention that:1) agitator is substituted with hole plate, material is set to be mixed in the form of meeting acetylene, acetone reaction rule and methyl butynol productive prospecting, the reaction time for ensureing to have abundance into all materials in auxiliary reactor and reaction rate faster, raising methyl butynol yield.2) device structure is simple, beneficial to industrially promoting.

Description

Auxiliary reactor for producing methyl butynol
Technical field
The present invention relates to ethynylation in a kind of production equipment of methyl butynol, especially a kind of methyl butynol production process Reaction unit used by step.
Background technology
Methyl butynol, CAS 115-19-5, molecular formula:C5H8O.It is mainly used as synthesis medicine and agricultural chemicals, terpenes is fragrant Material intermediate, acid inhibition inhibitor, viscosity stabiliser, viscosity reductant, nickel plating or copper-plated glazing agent etc..Also act as silicon rubber The polymerization inhibitor of middle platinum catalysis hydrosilylation.In addition it is also serving as being used as solvent, the stabilization of chlorinated solvents.
The method of industrial synthesizing methyl butynol mainly includes ethynylation and separates two steps.
Ethynylation step is that, with acetylene, acetone as raw material, solid (mostly powdered) potassium hydroxide is catalyst, or liquid hydrogen Sodium oxide molybdena makees catalyst, and ethynylation occurs in ethynylation device so as to ethynylation mixture is obtained.Its reaction equation is such as Under:
HC ≡ CH+NaOH=HC ≡ CHNaOH
The complex compound of generation and water decomposition, generate methyl butynol:
Separating step is then that separating-purifying goes out methyl butynol from ethynylation mixture, generally main to include flash distillation, saltout The steps such as dehydration, rectifying.
Fig. 1 illustrates the typical structure of ethynylation system, mainly mixed including stirred autoclave, auxiliary reactor and termination Clutch.In ethynylation step, the ethynylation of acetylene and acetone is generally carried out in stirred autoclave, in stirred autoclave, Alkynes, alcohol/ketone mixtures to lower and upper flowing, catalyst flow from top to bottom, mixed in the axial direction by density contrast, radially then lead The stirring action of agitator is leaned on to mix, because the temperature difference of reaction system, concentration difference are larger, therefore the methyl fourth in stirred autoclave The yield of alkynol is only capable of reaching 60% or so.To improve the yield of methyl butynol, conventional way is in stirring reaction at present One auxiliary reactor is set again after kettle, material is carried out primary first-order equation again in auxiliary reactor, so as to improve methyl butynol Yield.
Conventional auxiliary reactor structure is the reaction vessels such as the reactor with agitating device, reaction tower, reaction tube, its typical case Structure is as shown in fig. 1.In auxiliary reactor, unreacted material carries out hybrid reaction again in the presence of agitator, from And improve the yield of methyl butynol.Finally, the reaction stream in auxiliary reactor is passed through termination blender with reaction terminating agent Interior mixing and terminating reaction, obtain ethynylation mixture.After further being reacted by auxiliary reactor, the yield of methyl butynol is reachable To 85% or so.
The content of the invention
Further to improve the yield of methyl butynol, the invention provides a kind of anti-for producing the pair of methyl butynol Answer device.
The technical solution adopted in the present invention is:Auxiliary reactor for producing methyl butynol, including auxiliary reactor master Body, is communicated in the overflow pipe of auxiliary reactor lower body part, is communicated in the discharge nozzle of auxiliary reactor body top;It is characterized in that: Auxiliary reactor lower body part is provided with hole plate, and the overflow pipe is communicated on the wall below hole plate.
Can excessively cause side reaction generation dimethylhexyne glycol due to local acetone, it is as follows:
So the material in must assure that auxiliary reactor is sufficiently mixed uniformly, therefore the setting of agitator is considered as necessary 's.
By taking the ethynylation system of the methyl butynol shown in Fig. 1 as an example, it has been recognised by the inventors that limitation methyl butynol yield The problem of raising is essentially consisted in, in existing reaction system, material after initial reaction in stirred autoclave, by overflow pipe Into auxiliary reactor bottom, hybrid reaction is being carried out again under the immixture of agitator.As material is constantly from overflow pipe Flow into, material is gradually advanced from reactor lower part toward top in auxiliary reactor, and material constantly completes reaction during traveling, most Enter from upper outlet pipe eventually and terminate blender.In the process, because the stirring of agitator causes liquid acutely to disturb so that The product that auxiliary reactor top has carried out relatively fully reaction mixes with the unreacted material that bottom is newly entered from overflow pipe, makes product Thing is mixed into unreacted material, reduces the reaction rate of unreacted material.Also cause to have just enter into the unreacted of auxiliary reactor simultaneously Material quickly flow to auxiliary reactor top because of the violent flow-disturbing that stirring is formed, and the reaction that is not able to do in time also is just flowed into eventually from discharging opening Only blender.
On the other hand, in flinging auxiliary reactor from auxiliary reactor bottom into the material of auxiliary reactor from overflow pipe, shape Into the uneven fluid of flow velocity form bias current and dead angle in the reactor, it is impossible to ensure that all materials have in reactor and fill The reaction time of foot and faster reaction rate, while also increasing the degree of side reaction generation.
To solve the problems, such as the above, inventor cancels the agitator in auxiliary reactor, is replaced with hole plate so that from overflowing Flow tube flow into auxiliary reactor material by auxiliary reactor bottom hole plate stop, the fast fluid of flow velocity to both sides horizontal proliferation, And be formed down vortex and disturb, play the effect for being well mixed material.Then bottom material is past by the hole of hole plate Upper traveling, hole serves the effect for being uniformly distributed fluid, it is to avoid bias current and dead angle produce.Hole plate upper flow is upward simultaneously The unreacted material just entered from overflow pipe with hole plate bottom during propulsion is in opposing spaced apart state, and (fluid is acutely disturbed It is dynamic to be concentrated in hole plate bottom, it is ensured that hole plate upper flow is uniformly up advanced all the time, without flowing back to Hole plate bottom), the fluid that can be prevented effectively from the relatively fully reaction of auxiliary reactor top mixes with unreacted material, or newly Enter unreacted material and quickly flow to auxiliary reactor top.So as to ensure that all materials have the reaction of abundance in auxiliary reactor Time and quick reaction rate, and then realize improving the purpose of methyl butynol yield.
As a further improvement on the present invention, the overflow pipe is communicated in auxiliary reactor bottom part body, of the invention Mentality of designing, as long as being capable of achieving the purpose of the present invention on the side reaction wall that overflow pipe is communicated in below hole plate.But it is The material of hole plate bottom is set to mix evenly, and hole plate top material forms fluid evenly, preferably by overflow Pipe is communicated in auxiliary reactor bottom part body, and this also complies with the custom connected mode in industry.
As a further improvement on the present invention, the hole on the hole plate is can make the fluid by hole plate in hole Gap plate top produces the mode of disturbance to set.Hole on hole plate can with it is any be conducive to fluid to evenly distribute in the form of set Put, it is most typical such as equally distributed circular aperture, or other shapes aperture, and the or thin seam that uniformly or non-uniformly sets Etc. diversified forms.But in order that obtain still can be continuous during hole plate top is advanced after lower flow passes through hole plate There is the disturbance and mixing of appropriateness, further reduce local acetone excessively there is side reaction or form dead angle and bias current can Can, can be by the hole on hole plate can make to be set by way of hole plate top produces disturbance the fluid of hole plate Put.For example hole can be set to the inclined circular aperture that arranges according to certain rules, or likeness in form turbine blade shape Gap etc..So that fluid during through hole plate under the water conservancy diversion of hole hole plate top formed appropriate vortex or Disturbance, promotes hole plate upper flow further to mix.
As a further improvement on the present invention, the hole plate setting height(from bottom) be apart from auxiliary reactor bottom part body 15~ 40cm.The setting height(from bottom) of hole plate is too high or too low all to cause hole plate bottom material to be difficult to form stronger disturbance (for example Hole plate be installed on close to auxiliary reactor main body medium position even upper position when will be unable to realize the purpose of the present invention), Mixed effect is poor.Inventor draws through overtesting, it is generally the case that hole plate installation site and auxiliary reactor bottom part body Effect is preferable when distance is for 15~40cm.Additionally, the specific installation site of hole plate also with auxiliary reactor specification, overflow pipe material The factors such as flow velocity, flow are relevant.Therefore the number range is only preferred values under normal circumstances, and concrete numerical value scope can be according to reality Border situation is adjusted.
Additionally, due to general auxiliary reactor lower body part end socket welding position and auxiliary reactor bottom distance be about 20~ 30cm, therefore can be directly by hole plate weld in end socket weld, in order to the installation and plant maintenance of hole plate.
The beneficial effects of the invention are as follows:1) agitator is substituted with hole plate, makes material to meet acetylene, acetone reaction rule Form with methyl butynol productive prospecting is mixed, it is ensured that have the reaction of abundance into all materials in auxiliary reactor Time and faster reaction rate, methyl butynol yield reaches 95% or so in can making ethynylation mixture.2) device structure letter It is single, beneficial to industrially promoting.
Brief description of the drawings
Fig. 1 be in the prior art be used for produce methyl butynol ethynylation system structural representation.
Fig. 2 is auxiliary reactor structural representation of the invention.
Fig. 3 is the hole plate structure schematic diagram of embodiment one.
Fig. 4 is the hole plate structure schematic diagram of embodiment two.
Fig. 5 is a of Fig. 4 to fragmentary, perspective view.
Fig. 6 is the hole plate structure schematic diagram of embodiment three.
Fig. 7 is a of Fig. 6 to fragmentary, perspective view.
Marked in figure:1- stirred autoclaves, 2- auxiliary reactors, 21- auxiliary reactor main bodys, 3- terminates blender, and 4- overflows Flow tube, 5- discharge nozzles, 6- material feeding tubes, 7- catalyst charge pipes, 8- agitators, 9- hole plates, 9a, 9b, 9c- hole.
Specific embodiment
As shown in Figure 2 to 7, the auxiliary reactor for producing methyl butynol of the invention, including auxiliary reactor main body 21, the overflow pipe 4 of the bottom of auxiliary reactor main body 21 is communicated in, it is communicated in the discharge nozzle 5 on the top of auxiliary reactor main body 21;Side reaction The barrel diameter of device main body 21 is 800mm, is highly 1200mm, and end socket is highly 300mm, the weldering of the bottom head of auxiliary reactor main body 21 The place of connecing is provided with hole plate 9.
The present invention is further described with reference to the accompanying drawings and examples.
Embodiment one:
Fig. 2, Fig. 3 illustrate the first implementation method of the invention, the hole in the program on auxiliary reactor hole plate Structure is size, circular aperture arranged in a uniform, and the fluid for entering auxiliary reactor from overflow pipe is stopped by hole plate, in hole plate Bottom produces disturbance, is well mixed material.Then bottom material penetrates into hole plate by the uniform aperture on hole plate Top, is evenly distributed as uniform fluid by aperture, and upper flow is in opposing spaced apart with the fluid of hole plate bottom State.Uniform fluid is slowly advanced on hole plate top toward auxiliary reactor top, and step-reaction is complete in material traveling process, All materials have the residence time of abundance in auxiliary reactor, finally enter eventually from the discharging opening for being arranged at auxiliary reactor top Only blender, and mix terminating reaction with terminator, obtain ethynylation mixture.
Embodiment two:
Fig. 2, Fig. 4, Fig. 5 illustrate another embodiment of the invention, are not both with embodiment one, in the present embodiment Circular aperture on hole plate is arranged according to certain rules, and is inclined on hole plate in vertical direction, All of aperture is obliquely installed according to certain rule, makes hole plate that a flow guide system is integrally formed.Flow hole plate bottom The liquid stream of appropriateness disturbance is formed on hole plate top under the guide functions of multiple apertures when body is by hole plate, material is being worn To cross continue during being advanced toward auxiliary reactor top after hole plate and mix, further reduce the degree that side reaction occurs.
It should be understood readily by those skilled in this art that the present embodiment mesopore plate should possess certain thickness, to reach The purpose of this programme.
Embodiment three:
Fig. 2, Fig. 6, Fig. 7 illustrate the third implementation method of the invention, and the hole on the embodiment mesopore plate is Strip crevice, as shown in fig. 7, the strip crevice in the vertical direction is obliquely installed, and the water conservancy diversion slope with certain radian Road.The program can play effect and the effect similar with embodiment two.

Claims (6)

1. it is used to produce the auxiliary reactor of methyl butynol, including auxiliary reactor main body (21), is communicated in auxiliary reactor main body (21) overflow pipe (4) of bottom, is communicated in the discharge nozzle (5) on auxiliary reactor main body (21) top;It is characterized in that:Auxiliary reactor Main body (21) bottom is provided with hole plate (9), and the overflow pipe (4) is communicated on the wall below hole plate (9).
2. the auxiliary reactor for producing methyl butynol according to claim 1, it is characterised in that:The overflow pipe (4) it is communicated in auxiliary reactor main body (21) bottom.
3. the auxiliary reactor for producing methyl butynol according to claim 2, it is characterised in that:The hole plate (9) hole on is set with that can make the fluid hole plate (9) by way of hole plate (9) top produces disturbance.
4. the auxiliary reactor for producing methyl butynol according to claim 2, it is characterised in that:The hole plate (9) setting height(from bottom) is apart from auxiliary reactor main body (21) 15~40cm of bottom.
5. the auxiliary reactor for producing methyl butynol according to any claim in Claims 1 to 4, its feature It is:Hole on the hole plate (9) is circular port.
6. the auxiliary reactor for producing methyl butynol according to any claim in Claims 1 to 4, its feature It is:The hole plate (9) is installed on auxiliary reactor main body (21) bottom head weld.
CN201710149765.5A 2017-03-14 2017-03-14 Auxiliary reactor for producing methyl butynol Pending CN106824017A (en)

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Application Number Priority Date Filing Date Title
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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57132542A (en) * 1981-02-09 1982-08-16 Dainippon Ink & Chem Inc Continuous reactor
GB8321321D0 (en) * 1982-09-09 1983-09-07 Hri Inc Downwardly-directed fluid flow distribution system
US4603154A (en) * 1983-02-16 1986-07-29 Marathon Oil Company Method for preparing dilute polymer solutions
CN1125723A (en) * 1994-10-17 1996-07-03 拜尔公司 Process for the polynitration of aromatic compounds
CN1240202A (en) * 1998-05-29 2000-01-05 宇部兴产株式会社 Process and equipment for preparing dialkyl phenol
JP2000344804A (en) * 1999-03-31 2000-12-12 Mitsui Chemicals Inc Multi-stage gas-phase polymerization method and multi- stage gas-phase polymerization apparatus and apparatus to reduce the amount of entailed other components in polymer powder in multi-stage gas-phase polymerization apparatus
RU2247128C1 (en) * 2004-04-29 2005-02-27 Открытое акционерное общество "Воронежсинтезкаучук" Method of preparing neodymium-carboxylate component of diene hydrocarbon polymerization catalyst
US20080021242A1 (en) * 2006-07-19 2008-01-24 Michio Tanimoto Reactor for gas phase catalytic oxidation and a process for producing acrylic acid using it
CN102531270A (en) * 2010-12-28 2012-07-04 中国市政工程西北设计研究院有限公司 Multi-section multi-step anaerobic-oxic (AO) biological reaction tank
CN104056579A (en) * 2014-07-04 2014-09-24 华东理工大学 Gas and liquid distribution plate of up-flow reactor and inter-segment hydrogen supplementation device thereof
CN206577740U (en) * 2017-03-14 2017-10-24 四川泸州巨宏化工有限责任公司 Auxiliary reactor for producing methyl butynol

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57132542A (en) * 1981-02-09 1982-08-16 Dainippon Ink & Chem Inc Continuous reactor
GB8321321D0 (en) * 1982-09-09 1983-09-07 Hri Inc Downwardly-directed fluid flow distribution system
US4603154A (en) * 1983-02-16 1986-07-29 Marathon Oil Company Method for preparing dilute polymer solutions
CN1125723A (en) * 1994-10-17 1996-07-03 拜尔公司 Process for the polynitration of aromatic compounds
CN1240202A (en) * 1998-05-29 2000-01-05 宇部兴产株式会社 Process and equipment for preparing dialkyl phenol
JP2000344804A (en) * 1999-03-31 2000-12-12 Mitsui Chemicals Inc Multi-stage gas-phase polymerization method and multi- stage gas-phase polymerization apparatus and apparatus to reduce the amount of entailed other components in polymer powder in multi-stage gas-phase polymerization apparatus
RU2247128C1 (en) * 2004-04-29 2005-02-27 Открытое акционерное общество "Воронежсинтезкаучук" Method of preparing neodymium-carboxylate component of diene hydrocarbon polymerization catalyst
US20080021242A1 (en) * 2006-07-19 2008-01-24 Michio Tanimoto Reactor for gas phase catalytic oxidation and a process for producing acrylic acid using it
CN102531270A (en) * 2010-12-28 2012-07-04 中国市政工程西北设计研究院有限公司 Multi-section multi-step anaerobic-oxic (AO) biological reaction tank
CN104056579A (en) * 2014-07-04 2014-09-24 华东理工大学 Gas and liquid distribution plate of up-flow reactor and inter-segment hydrogen supplementation device thereof
CN206577740U (en) * 2017-03-14 2017-10-24 四川泸州巨宏化工有限责任公司 Auxiliary reactor for producing methyl butynol

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