CN102898302A - Water separating system - Google Patents
Water separating system Download PDFInfo
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- CN102898302A CN102898302A CN201210242576XA CN201210242576A CN102898302A CN 102898302 A CN102898302 A CN 102898302A CN 201210242576X A CN201210242576X A CN 201210242576XA CN 201210242576 A CN201210242576 A CN 201210242576A CN 102898302 A CN102898302 A CN 102898302A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
- B01J2219/00792—One or more tube-shaped elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00867—Microreactors placed in series, on the same or on different supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00905—Separation
- B01J2219/00907—Separation using membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00954—Measured properties
- B01J2219/00957—Compositions or concentrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00954—Measured properties
- B01J2219/00959—Flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00954—Measured properties
- B01J2219/00961—Temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00954—Measured properties
- B01J2219/00963—Pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00968—Type of sensors
- B01J2219/0097—Optical sensors
- B01J2219/00975—Ultraviolet light
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00952—Sensing operations
- B01J2219/00968—Type of sensors
- B01J2219/0097—Optical sensors
- B01J2219/00977—Infrared light
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention provides a water separating system with simple device structure which can improve water separating efficiency and can set reaction time freely. Water separating system for separating water from a product solution obtained after the chemical reaction of reactants, comprises a mixing device (3) for mixing the supplied reactants, a device for performing a chemical reaction, which is connected to mixing device to chemically convert the mixed reactants, a device for separating water, which is connected to the mixing device for performing the chemical reaction, for separating the water formed in the device for performing the chemical reaction, and a controlling unit (12) for controlling a chemical reaction time. Water separating system (100) for separating water from a product solution obtained after the chemical reaction of reactants, comprises a mixing device (3) for mixing the supplied reactants, a device for performing a chemical reaction, which is connected to the mixing device to convert the mixed reactants chemically, a device for separating water, which is connected to the mixing device for performing the chemical reaction, for separating the water formed in the device for performing the chemical reaction, and a controlling unit (12) for controlling a chemical reaction time in the device for performing the chemical reaction. The controlling unit is designed so that the controlling unit shortens the chemical reaction time of the device for performing the chemical reaction, when a large product amount in the solution is discharged from the device for performing the chemical reaction, and extends the chemical reaction time of the device for performing the chemical reaction, when a small product amount in the solution is discharged from the device for performing the chemical reaction.
Description
Technical field
The present invention relates to water separating system.
Background technology
In recent years, by the making such as micro-processing technology, the device of mixed stream is that so-called microreactor is used to each field such as biology, medical field, chemosynthesis in fine channel.Feature as the reaction of using microreactor can list for example miniaturization of reaction system.By the miniaturization of this reaction system, the molecule (that is, raw molecule) of formation fluid spreads rapidly and mixes, so relatively increase with respect to the surface-area of volume.Its result compares with rhythmic reaction, and reaction efficiency improves, and therefore expects Reaction time shorten and improves yield etc.
A kind of as chemical reaction has balanced reaction.So-called balanced reaction is in reversible reaction, and along with reaction is carried out, the speed of response of positive dirction and backward speed of response become equal, and the ratio of components of raw material and resultant looks not have vicissitudinous reaction.
The a kind of of balanced reaction has as resultant except the purpose resultant, also generates the reaction of water.Particularly, make alcohol and the esterification of carboxylic acid reaction etc. such as enumerating.At this moment, the purpose resultant is carboxylicesters.This reaction is balanced reaction, and therefore, the purpose resultant of generation (for example, carboxylicesters etc.) is owing to the water that generates simultaneously is hydrolyzed, and returns initial feed (for example, carboxylic acid etc.).That is, positive reaction and reversed reaction are carried out simultaneously.
When carrying out this balanced reaction, compare in the situation about being exceedingly fast with the speed that the purpose resultant is hydrolyzed in the speed that generates the purpose resultant, can not produce large problem with the viewpoint of common yield.Yet, in the situation such as slightly fast, even the purpose resultant generates, also be hydrolyzed immediately, so often be difficult to improve the yield of purpose resultant than the latter's speed in the former speed.
Therefore, in order to improve the yield of this reaction, consideration will separate (removing) with the produced simultaneously water of purpose resultant outside reaction system.By such operation, the chemical equilibrium deflection generates the direction of purpose resultant, can improve yield.
As the technology of from the mixing solutions that comprises above-mentioned such purpose resultant and water, separating (removing) water, since Gu, used the distilled method.In addition, in recent years, except the distilled method, soak into vaporization (pervaporation) method and receive much concern.Soak into gasification for using and separate object material (such as water etc.) has the method for the separatory membrane of affinity.As the concrete usability methods of separatory membrane, one-sided (supply side) configuration (or circulation) mixing solutions at separatory membrane maintains decompression state with opposition side (seeing through side).Thus, see through easily the vaporize that arrives the liquid of opposition side in the separatory membrane, utilize the penetration speed of each composition poor, the separate object material permeance is separated.
Various researchs have been carried out for the isolation technique of having utilized the water that soaks into gasification.For example, put down in writing in the patent documentation 1 and had an end obturation and the separatory membrane of the tubulose that the other end is opened, on the tube sheet that is arranged on the sleeve pipe, fix the other end of above-mentioned separatory membrane in the water-lute mode, the film module that makes liquid mixture or the desired substance in the gaseous mixture in the circulation of the outside of above-mentioned separatory membrane selectively see through the inboard of this separatory membrane, the i.e. film module of the space filling Porous compaction material between the outside of the inboard and above-mentioned separatory membrane that is formed at above-mentioned sleeve pipe.
In addition, for example, put down in writing the film separation reaction system in the patent documentation 2, it possesses reaction unit, to in above-mentioned reaction unit, generate and be mingled with the film module that composition separates with this material composition with material composition evaporates simultaneously, to the above-mentioned vaporized blend heated heating unit that is mingled with composition and material composition, and the circulation device that makes steam pump circulation in the liquid phase of above-mentioned reaction unit of the material composition that is separated by above-mentioned film module, the separatory membrane of above-mentioned film module is made of zeolite membrane, and above-mentioned heating unit is to above-mentioned raw materials composition and above-mentioned composition not condensing and mode degree that exist with steam condition in above-mentioned film module that is mingled with are consisted of with heat supply.
The prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2007-203210 communique
Patent documentation 2: No. 4462884 communique of Japanese Patent
Summary of the invention
Invent problem to be solved
In the technology of patent documentation 1 record, how much water that is contained in solution (reaction solution) all carries out lock out operation.Therefore, has the water yield because comprising, the situation that the separation efficiency of water is low.Therefore, for Separation of Water, sometimes need lock out operation repeatedly.
Also have, in the technology of patent documentation 1 record, because needs are warming up to the transpirable temperature of solution, so equipment maximizes sometimes.
In addition, in the technology of patent documentation 2 record, from reaction solution, make the evaporation of raw material (ethanol) and water, make it by having the film module of separatory membrane, carry out moisture from.Then, only with moisture from after raw material return reaction vessel.Like this, in the technology of patent documentation 2 records, need to be for separating of the water circuit cycle.Therefore, in this technology, sometimes for forming loop cycle, equipment enlarging or complicated.In addition, sometimes also need be used to the equipment that makes the reaction solution evaporation, equipment enlarging.
Have again, the impact of (returning in the reaction vessel) raw material that is circulated, the temperature with reaction solution is controlled unsettled situation.Its result is difficult to control the reaction in the reaction vessel, has yield and reduces, or generate the situation of by product.In addition, certain because leaving the time of beginning to moisture after raw material and the water evaporation, so only have by the change cycle index, could control the reaction times.That is, has the situation that the control in reaction times is restricted.
The present invention finishes in view of above-mentioned problem, and its purpose is, provide with easy equipment to consist of the separation efficiency that can improve water, but the water separating system in Set arbitrarily reaction times.
In order to solve the means of problem
The inventor etc. are in order to solve found that of the wholwe-hearted research of above-mentioned problem, are controlled to the time that the separation of water begins by the amount based on resultant, can solve above-mentioned problem, have finished the present invention.
The invention effect
According to the present invention, can provide easily equipment to consist of, improve the separation efficiency of water, water separating system that can the Set arbitrarily reaction times.
Description of drawings
Fig. 1 is the figure that schematically shows the formation of the water separating system that the first embodiment relates to;
Fig. 2 is the figure that schematically shows the formation of the water separation device that is applicable to the water separating system that the first embodiment relates to;
Fig. 3 is explanation figure about the velocity constant of the reaction carried out in the water separation device that the first embodiment relates to;
Fig. 4 is that expression is with respect to the coordinate diagram of the velocity variations of time;
Fig. 5 is the figure that schematically shows the formation of the water separating system that the second embodiment relates to;
Fig. 6 schematically shows the figure that the chemical reaction that applies to the water separating system that the second embodiment relates to carries out the formation of equipment;
Fig. 7 is the flow process when improving moisture that the second embodiment relates to from the control of efficient;
Fig. 8 is the figure that schematically shows the formation of the water separating system that the 3rd embodiment relates to;
Fig. 9 is the result's of expression embodiment coordinate diagram.
Nomenclature
3 mix with microreactor (mixing device)
4 chemical reactions carry out section (chemical reaction carries out device)
5 temperature adjusters (chemical reaction temperature control device)
6 moisture are from using microreactor (water separation device)
7 moisture are from temperature-control device
12 control device (operating device)
13 chemical reactions carry out equipment
15 determinators (on-line determination device)
Embodiment
Below, the limit is used for implementing mode of the present invention (present embodiment) with reference to accompanying drawing limit explanation, and present embodiment is not subjected to any restriction of following content, can at random change within not breaking away from aim scope of the present invention and implements.
(1. the first embodiment)
(formation)
Fig. 1 is the figure that schematically shows the formation of the water separating system 100 that the first embodiment relates to.Water separating system 100 shown in Figure 1 is to be the water separating system of resultant solution (reaction soln) Separation of Water that obtains behind oleic acid and the methyl alcohol chemical reaction from making raw material.In addition, in the first embodiment, use oleic acid and methyl alcohol as the concrete example of raw material, but so long as generate the composition of water by chemical reaction, then be not limited to these.
In addition, the details aftermentioned is used oleic acid and methyl alcohol and is carried out in the situation of chemical reaction (specifically esterification) Witconol 2301 and water generation as raw material.Therefore, the composition beyond dewatering in the composition that generates in the present embodiment is called " resultant ".Therefore, the resultant of the first embodiment is " Witconol 2301 ".
Mixing with microreactor 3 (mixing device) is the device that mixes oleic acid and methyl alcohol.That is, supply oleic acid and methyl alcohol mix in mixing with microreactor 3.Concrete formation as mixing with microreactor 3 is not particularly limited, as long as rapid mixing raw material.For example, as the stream shape of mixing with microreactor 3, can be Y-shaped, T font, form the shape of multilayer stream etc., also can use commercially available microreactor.
In addition, in the first embodiment, although with mixing with microreactor 3 two kinds of raw materials are mixed, the raw material more than three kinds is mixed.For example, in the situation that three kinds of raw materials are mixed, replace mixing with microreactor 3, mixing microreactor with the stream that makes three kinds of raw materials mixing can be set, also can be connected in series a plurality of mixing microreactors that two kinds of raw materials are mixed, thereby raw material is mixed, the raw material of the kind (quantity) of hope is mixed.
The degree of mixing with the mixing in the microreactor 3 in addition, has no particular limits.In addition, raw material both can evenly mix each other, also can not mix and inhomogeneous (so-called emulsified state).
Mixing has no particular limits with the representative length in the stream path of microreactor 3.But, from effectively utilizing to greatest extent the viewpoint of the effect of micron-sized reaction, preferably below several mm, from the viewpoint that raw material is mixed rapidly, more preferably tens of μ m～1mm.
As the material that consist of to mix with microreactor 3, only otherwise the chemical reaction that impact produces then can use arbitrarily material.As such material, such as listing stainless steel, silicone, gold, glass, hastelloy, silicone resin, fluorine resin etc.In addition, in addition, also can use lass lining, at the material of metallic surface coating nickel or gold etc. and make the material that solidity to corrosion is improved of material etc. of the surface oxidation of silicone.But, from heat conductivity and intensity viewpoint, preferably use metal as consisting of the material that mixes with microreactor 3.
In addition, carry out in the section 4 in order to react rapidly at chemical reaction described later, arrange and mix with microreactor 3, further, also can not shown temperature adjuster be set to connecting the pipe arrangement that mixes with microreactor 3 and pump 2a or pump 2b, to mix in the temperature of regulation.Thus, increasing extent of temperature or the cooling extent of the reaction soln of section 4 can be reduced to carry out at chemical reaction, chemical reaction can be carried out more expeditiously.
Chemical reaction carries out section 4 (chemical reaction carries out device) makes the raw material that has mixed in mixing with microreactor 3 carry out the device of chemical reaction.Reaction soln (that is, the mixture of oleic acid and methyl alcohol) carries out section's 4 performance functions from mixing the pipe arrangement (fine channel) of discharging rear circulation with microreactor 3 as chemical reaction in the first embodiment.Therefore, the length that chemical time can be by changing this pipe arrangement and the section area of stream are controlled.
At this, above-mentioned " chemical time " is strictly speaking after mixing is mixed with each other with microreactor 3 interior raw materials, arrives to moisture from supplying with microreactor 6 (aftermentioned), and water begins the separated time.But, also short more a lot of than the time of carrying out section's 4 interior delays at chemical reaction in the time of mixing with microreactor 3 interior delays.In addition, in fact also carry out chemical reaction at moisture in microreactor 6, as described later, because of water separated time the, the balanced deflection of chemical reaction, so compare with chemical reaction, sepn process one side of water preferentially carries out.Therefore, " chemical time " in this specification sheets namely is illustrated in chemical reaction and carries out residence time in the section 4.
In addition, also can fix the length of above-mentioned pipe arrangement, control is controlled above-mentioned chemical time thus to mixing with the oleic acid of microreactor 3 supplies and the amount of methyl alcohol.That is, length and the internal diameter of pipe arrangement are certain, so that in the situation of a large amount of reaction soln circulation, carry out the time that section 4 is detained at chemical reaction and shorten.On the other hand, make in the situation of a small amount of reaction soln circulation, the time of carrying out section's 4 delays at chemical reaction is elongated.So, utilize such relation, also can control chemical time.In addition, in this situation, can be undertaken by control device 12 described later to the control of the liquor charging flow that mixes the raw material of supplying with microreactor 3.
In addition, have no particular limits for the material that consists of chemical reaction and carry out section 4, for example, can use with mixing with the same material of microreactor 3 to consist of.In addition, such as also using the pipe that consisted of by materials such as Teflon (registered trademark) etc.In addition, the stream path of carrying out section 4 for chemical reaction also is not particularly limited, and for example, also can be applied in the stream path of mixing with explanation in the microreactor 3.
Temperature adjuster 5 (chemical reaction temperature control device) is the device of the temperature of control chemical reaction when carrying out the chemical reaction of section 4.The concrete formation of temperature adjuster 5 has no particular limits, such as the thermostatic bath that can use fluids such as utilizing water, water-ethanol mixed solvent, ethylene glycol, Peltier's element (Pelti er dev i ce), bell-type electricradiator etc.In addition, be in the situation of room temperature degree in chemical reaction temperature, according to the thermal control of reaction heat and microreactor, also set temperature is not regulated machine 5.
Moisture is from microreactor 6 (water separation device) being the device that is separated in the water in the reaction soln that chemical reaction carries out section 4 circulation.Consist of moisture and have no particular limits from material and stream path with microreactor 6, for example, can be applied in equally the content of mixing with explanation in the microreactor 3.
In addition, moisture also can be connected in series setting more than two from also can only arranging one with microreactor 6.These disengaging times according to the water of hope can suitably be set.In addition, with reference to Fig. 2, moisture is from having as described later point-symmetric structure with microreactor 6, so even be connected in series in the plural situation, a plurality of moisture also can be set from using microreactor 6 in minimal space.
At this, the limit describes from the concrete formation with microreactor 6 with reference to the moisture of Fig. 2 limit to the first embodiment.
Shown in Fig. 2 (a), moisture is from having roughly barrel shape with microreactor 6, and its upper and lower end parts possesses flange sample parts.And, be provided with influx 20b that reaction soln flows into, relief outlet 20d (with reference to Fig. 2 (b)) that water is discharged from these flange sample parts, discharge the relief outlet 20e for the treatment of solution behind the reaction soln Separation of Water.
Moisture is from being the structure shown in Fig. 2 (b) with microreactor 6 inside.Shown in Fig. 2 (b), moisture is same structure from the upper and lower end parts with microreactor 6.Therefore, for the purpose of simplifying the description, mainly the structure of upper end and sidepiece described.
Moisture is from main by comprising that the first disc parts 20, the second disc parts 21 that possesses jut 21a that possesses influx 20b, 20c, the microreactor main body 22 that comprises flange portion 22a and cylinder part 22b cylindraceous consist of with microreactor 6.And the first disc parts 20 and the second disc parts 21 and flange portion 22a are fastening by the screw 20a that connects them (among Fig. 2 6).
In addition, between the first disc parts 20 and the second disc parts 21, be provided be used to the gasket that prevents leakage (zero type circle) 23a, 23b.In addition, be provided with too gasket 23c between the second disc parts 21 and the flange portion 22a.
Separatory membrane 24 is films of Separation of Water from reaction soln.The separatory membrane 24 of the first embodiment uses T-shaped zeolite membrane.Separatory membrane 24 is via not shown gasket, and the mode on every side of jut 21a arranges to surround up and down.In addition, gasket also can be arranged in the mode with the second disc parts 21 compressions the upper and lower end parts of separatory membrane 24.By like this, can prevent leakage.
And, be formed at the reaction soln stream 25 that space between the inner-wall surface of the outside of separatory membrane 24 and cylinder part 22b becomes the reaction soln circulation.In addition, the space that is formed at the inboard of separatory membrane 24 becomes the state by reliever 11 (aftermentioned) decompression.Therefore, water becomes water vapor and sees through separatory membrane 24 and discharge (being described in detail later) to the outside.That is, the inner space of separatory membrane 24 becomes the water vapor stream 26 of water vapor circulation.
In addition, influx 20b and reaction soln stream 25, the hole (not shown) that reaction soln stream 25 and relief outlet 20e uniformly-spaced arrange via the circumferential direction at the second disc parts 21 and being communicated with.By such hole is set, can make reaction soln spread all over moisture from the region-wide equably circulation in the inside of microreactor 6, can prevent from occuring through circulation (so-called short circuit) on the road that the pressure-losses reduces.
In addition, water vapor stream 26 and relief outlet 20d same (as shown) are communicated with.Therefore, the water that is contained in the above-mentioned reaction soln that circulates in reaction soln stream 25 by influx 20b is discharged to the outside by water vapor stream 26 and relief outlet 20d through separatory membrane 24.On the other hand, the treatment solution (that is the liquid that, comprises Witconol 2301) of water after separated from above-mentioned reaction soln discharged to the outside by relief outlet 20.
In addition, the moisture of the first embodiment is sealed from the influx 20c with microreactor 6.But, as above-mentioned, moisture from microreactor 6 with near the above-below direction center as symmetric points, have point-symmetric formation.Therefore, connecting a plurality of moisture from using in the situation of microreactor 6, changing in the situation of above-below direction use, as required, also can not carry out above-mentioned sealing, perhaps seal different influxs or relief outlet.
In addition, each influx and relief outlet consist of in pipe (pipe arrangement) attachable mode.Particularly, be formed with the screw hole (not shown) that assembles usefulness at each influx and relief outlet, by using not shown assembly parts, can be at each influx and relief outlet pipe connecting.
Return Fig. 1, the integral body that goes on to say water separating system 100 consists of.
Temperature adjuster 7 (moisture is from temperature-control device) is the device of control moisture from the temperature of using microreactor 6.That is, be the device of control temperature during Separation of Water from reaction soln.The concrete formation of temperature adjuster 7 has no particular limits, and for example, also can use the device same with above-mentioned temperature adjuster 5.
In addition, in the first embodiment, the temperature during the separating of the temperature in the time of can being set as chemical reaction and water is different.For example, temperature that can be when improving chemical reaction, the mode design temperature of the temperature when reducing the separation of water is regulated machine 5,7.Chemical reaction does not carry out when not surpassing activation energy, so the high side of temperature of reaction easily reacts.On the other hand, separatory membrane 24 (with reference to Fig. 2) preferably carries out the separation of water because thermotolerance is not too high usually at low temperature.Therefore, temperature adjuster 5,7 is set like this, the temperature during the separating of the temperature in the time of can making chemical reaction and water is different.
Back pressure valve 8 is valves that the reaction soln stream 25 that illustrated with reference Fig. 2 and relief outlet 20e are connected.By back pressure valve 8 is set, make reaction soln stream 25 form pressurized state, can prevent the vaporization of low-boiling methyl alcohol.Its result, the pressure reduction of reaction soln stream 25 and water vapor stream 26 increases, and can promote the separation of the water due to the separatory membrane 24.But, all be set in the boiling point of oleic acid and methyl alcohol at temperature adjuster 5,7 design temperature and compare, enough in the situation of low temperature, also can not establish back pressure valve 8.
Cold-trap 10 is devices that the water vapor stream 26 that illustrated with reference to Fig. 2 limit with the limit and relief outlet 20d are connected.That is,, become the water that water vapor discharges to the outside and be cooled at cold-trap 10 from separated with microreactor 6 at moisture.Thus, the water of vaporization (water vapor) becomes the water of liquid, can easily reclaim separated water.
By control device 12, the control chemical reaction carries out the chemical time of section 4.Particularly, control device 12 is by control pump 2a, 2b, and control is to the liquor charging flow that mixes with the raw material of microreactor 3.Thus, as above-mentioned, the control chemical time.At this moment, control device 12 carries out the control of the liquor charging flow of raw material based on the ratio of the resultant in the treatment solution that flows into resultant case 9.That is, carry out feedback control.
Particularly, carry out following control: when the amount of the resultant in treatment solution (Witconol 2301) is many, shorten chemical time, when the amount of resultant is few, prolong chemical time.In other words, carry out following control: carry out Witconol 2301 amount that section 4 discharges when many from chemical reaction, shorten the chemical time that chemical reaction carries out section 4, carry out the amount of the Witconol 2301 that section 4 discharges when few from chemical reaction, prolong the chemical time that chemical reaction carries out section 4.
The reason of carrying out this control is described.As above-mentioned, for the liquor charging flow of control raw material, so control device can be predicted the growing amount of Witconol 2301.Then, the amount of the growing amount of comparison prediction and the actual Witconol 2301 that generates in the amount situation still less than prediction, is judged as and can carries out further chemical reaction, prolongs chemical time.Thus, can generate more Witconol 2301 and water.
On the other hand, amount at the growing amount of the Witconol 2301 of predicting and the actual Witconol 2301 that generates is in the situation of roughly the same degree, prolong chemical time even judge more than this, the growing amount of Witconol 2301 does not increase yet, and shortens at leisure the control of chemical time.By such control, can save the waste of chemical time.
The measuring method of the growing amount of Witconol 2301 has no particular limits, and for example, can use density, specific refractory power, FT-IR (Fourier Transform-I nfrared, Fourier transform type infrared spectroscopy), UV (Ultraviolet; The ultraviolet ray light splitting), HPLC (High Performance Liquid Chromatography; High performance liquid chromatography (HPLC)), GC (Gas Chromatography; Gas-chromatography) etc. measure.
In addition, control device 12 also has the function of control temperature adjuster 5,7 driving.That is, when regulating machine 5,7 design temperature to control device 12 input temps, control device 12 is controlled temperature adjuster 5,7 in the mode that is adjusted to this design temperature.
In addition, control device 12 is such as utilizing the realizations such as CPU (Central Processing Unit), sequencer.
(action effect)
Below, the limit is with reference to the action effect of Fig. 3 and Fig. 4 limit explanation water separating system 100.
As shown in Figure 3, at the supply side (being reaction soln stream 25) of separatory membrane 24, positive reaction is with reaction velocity constant k
1, reversed reaction is with the speed of response k that fixes a number
-1Carry out balanced reaction.In addition, more strictly speaking, react to the Witconol 2301 of emanating after just having mixed from raw material, at this for convenience of description, be defined as at moisture from representing with the reaction in the microreactor 6.And the water of the liquid of supply side is depressurized becomes water vapor through separatory membrane 24, arrives and sees through side (being water vapor stream 26).Penetration speed constant (velocity of separation constant) when water is seen through separatory membrane 24 is set as k
2
As shown in Figure 4, the reaction times is longer, and according to the residual content of raw material, the speed of response of positive reaction (positive reaction speed) is lower.In addition, the reaction times is longer, owing to react, the amount of the water that exists in the reaction system more increases.On the other hand, for the separation of the water that is undertaken by separatory membrane 24, the amount of the water in the reaction soln is more and more, and velocity of separation is accelerated.If consider these, the reaction times needs only sufficiently long, and it is more that the amount of the water that exists in reaction system just becomes, so the velocity of separation of water is accelerated.
But, in the situation of balanced reaction, carry out simultaneously reversed reaction with positive reaction, the reaction times is longer, and the speed of response of reversed reaction is faster on the contrary.Therefore, even merely guarantee the long reaction times, during the time of certain degree of process, the speed of response of positive reaction becomes identical with the speed of response of reversed reaction, is difficult to react.In other words, the formation speed of water reduces at leisure, and the amount of the water that exists in reaction system reaches maximum value.Therefore, as water separating system 100, suitably set the reaction times by the amount according to resultant, can realize the high separating efficiency (being high yield) of water and leave the minimizing of the dead time of beginning to moisture.In addition, because do not make reaction solution circulation, so complicated and maximization that can suppression equipment etc.In addition, because can stablize the temperature control of carrying out reaction solution, so can suppress the generation of by product.
(2. the second embodiment)
Below, the limit illustrates the water separating system 200 of the second embodiment with reference to Fig. 5 limit.In addition, to marking identical symbol with water separating system 100 identical devices (parts) shown in Figure 1, omit its detailed explanation.
(formation)
As shown in Figure 5, in water separating system 200, chemical reaction carry out section 4 by three chemical reactions carry out equipment 131,132,133 and three stream control device 141,142,143 consist of.Fig. 6 (a) expression chemical reaction carries out the structure of equipment 13.
It is the devices that are embedded in fine channel 13b inside, that have specified length of base material 13d that chemical reaction carries out equipment 13.The end of fine channel 13b arranges opening as influx 13a in face side shown in Fig. 6 (a), the other end overleaf side arranges opening as relief outlet 13c.Therefore, the reaction soln that flows into from influx 13a flows through fine channel 13b, discharges from relief outlet 13c.
Consist of chemical reaction and carry out the material of equipment 13 there is no particular limitation, for example, can use with above-mentioned and mix with the same material of microreactor 3.In addition, consist of the representative length in stream path that chemical reaction carries out the fine channel 13b of equipment 13 and also have no particular limits, for example, can with above-mentioned mix with the stream path of microreactor 3 same.
In addition, the stream shape of fine channel 13b is not limited to the shape shown in Fig. 6 (a), for example, also can be linearity, spirrillum etc.In addition, also can carry out equipment 13 to each chemical reaction and set different stream shapes.In addition, also can be that a part is identical, remainder is different.But, from make chemical reaction carry out equipment 13 except thermal characteristics even, this viewpoint of chemical reaction easy to control, preferred whole chemical reaction carries out equipment 13 and has identical shaped fine channel 13b.In addition, chemical reaction carries out equipment 13 both can form integrated formation, also can form the formation that can decompose.
In addition, the position of the position of influx 13a and relief outlet 13c is carried out the length direction center of equipment 13 take chemical reaction point-symmetric mode is arranged as symmetric points form.And, by influx 13a and relief outlet 13c are set like this, shown in Fig. 6 (b), by overlapping simply, can easily change the length of fine channel 13b.And, dead volume can be formed inferior limit and connect plural chemical reaction and carry out equipment 13.
In addition, be formed with the screw hole (not shown) that assembles usefulness at influx 13a and relief outlet 13c.Therefore, by using not shown assembly parts, pipe is connected with influx 13a and relief outlet 13c.
In water separating system shown in Figure 5 200, a chemical reaction carries out equipment 13 and interconnects via stream control device 14.And, switching stream control device 14 by control device 12, the chemical reaction that can change the reaction soln circulation carries out the quantity of equipment 13.Therefore, carry out section 4 by such formation chemical reaction, can easily change the length of fine channel 13b, can be easy to control the time of chemical reaction.
Particularly, for example wanting to make a chemical reaction to carry out in the situation of equipment 13 (131) circulations, control flow rate control device 141,143 makes mixture not arrive chemical reaction and carries out equipment 132,133 and get final product.Wanting to make two chemical reactions to carry out equipment 13 (in 131,132,133 two) or three chemical reactions carry out in the situation of equipment 13 (131,132,133) circulation, equally, by control stream control device 14, can easily change.That is, by control stream control device 14, can more easily change the length of the fine channel 13b of circulation.
In addition, as stream control device 14, can valve be set at each stream, by controlling these valves, the stream of control circulation.In addition, in Fig. 5, chemical reaction carries out equipment more than 13 and is connected in series and represents, carries out equipment 13 and consists of but also can only connect a chemical reaction.
(control method)
Below, the limit is with reference to the control method of Fig. 7 limit explanation water separating system 200 shown in Figure 5.In addition, the control in the flow process shown in Figure 7 is undertaken by control device 12.In addition, whether the separation efficiency of water improves, and judges according to the variation of the growing amount of Witconol 2301.That is, the chemical quantity of the growing amount of Witconol 2301 and water is theoretical than being 1:1, improves so the growing amount of Witconol 2301 improves the separation efficiency (more specifically, the formation efficiency of water) of expression water.
Behind step S 102, begin the research (step S 101) for the separation efficiency raising of water.At first, when mixing with the flow (that is, the reaction times of regulation) of the regulation that preseted oleic acid and methyl alcohol (step S 102), the beginning chemical reaction, Witconol 2301 and water generate.Amount according to the Witconol 2301 that at this moment generates is calculated the separation efficiency of water, compares with theoretical efficiency.Its result, improve in the separation efficiency of judging water outlet (that is, and in the situation well) (step S103 is), reaction times realization the best, (step S110, S111) finished in research, continues to move in this condition.
On the other hand, in step S103, do not thinking (S103 in the situation that the separation efficiency of water improves, no), (step S104 is) control pump 2a, 2b change liquor charging flow in oleic acid and the modifiable situation of methyl alcohol liquor charging flow, repeating step S102 and step S103.If can not change in the situation of liquor charging flow (step S104, no; For example, although want to increase the liquor charging flow, pump 2a, 2b are with situation of maximum output services etc.), carry out the setting (step S105) that chemical reaction carries out equipment 13.
Particularly, control stream control device 14 determines that the chemical reaction of circulation carries out the quantity of equipment 13.Thus, again carry out the setting of chemical time.Then, chemical reaction carries out the setting of equipment 13 to be finished, and above-mentioned steps S103 is same, (step S106 when the separation efficiency of judgement water outlet is good, be), (step S110, S111) finished in the research of reaction times realization optimizing, continues operation under this condition.
In step S106, in the low situation of the separation efficiency of water (step S106, no), the chemical reaction of change circulation carries out the quantity (step S107 is) of equipment 13, repeating step S105 and step S106.On the other hand, in step S107, can not change chemical reaction and carry out in the situation of equipment 13 (step S107, no; For example, although want to prolong chemical time, used whole chemical reactions to carry out the situation etc. of equipment 13), control temperature adjuster 7, the separation temperature (step S108) of change water.Then, thus, judge whether the separation efficiency of water improves (step S109), in situation about improving, research finishes (step S109 is step S110, step S111).
Do not think in step S109 (step S109, no) in the situation that separation efficiency improves that the separation temperature of research water is variable (step S112) whether, in the modifiable situation, repeating step S108 and step S109.On the other hand, for example, even wanting to improve separation temperature, but temperature adjuster 7 is with in the situation of maximum output running and to reach the situation of heat resisting temperature boundary of separatory membrane 24 inferior, separation temperature can not the situation of change under, can not realization response time optimal, research end (step S112, no, step S113, step S111)
(3. the 3rd embodiment)
Below, the limit illustrates the water separating system 300 of the 3rd embodiment with reference to Fig. 8 limit.In addition, to Fig. 1 and water separating system 100 shown in Figure 5, symbol that 200 identical device (parts) marks are identical, omit its detailed explanation.
(formation)
In water separating system 300, be provided with the determinator 15 (on-line determination device) of automatically measuring resultant (Witconol 2301) amount.In this embodiment, determinator 15 is arranged between back pressure valve 8 and the resultant case 9, but also can be arranged at moisture from using between microreactor 6 and the back pressure valve 8.
The concrete formation of determinator 15 has no particular limits, and for example, uses and utilizes the apparatus for automatically measuring of aforesaid method to get final product.And by such determinator 15 is set, the operator need not manually measure the amount of the resultant in the treatment solution, can avoid the complexity of controlling.And the amount of the resultant of mensuration is input control device 12 immediately, therefore, can greatly reduce the time lag when carrying out above-mentioned feedback control.Therefore, can improve more accurately the separation efficiency of water.
(embodiment)
Below, to enumerate embodiment and illustrate in greater detail present embodiment, present embodiment is not subjected to any restriction of following embodiment.
Use oleic acid and methyl alcohol, study the separation efficiency of the water that generates with Witconol 2301.At this moment, use water separating system 100 shown in Figure 1.Below, detailed condition is shown.
(embodiment 1)
(formation)
As methyl alcohol, the methyl alcohol of the reagent superfine of the pure pharmaceutical worker's industry of use and light society system.In addition, the methyl alcohol that uses in an embodiment uses the methanol solution that obtains as the catalyst mix vitriol oil (with the pure pharmaceutical worker's industry of light society system, reagent is superfine).The combined amount of the vitriol oil all is 1.6 quality % with respect to methanol solution.
As oleic acid, use and the pure pharmaceutical worker of light already society system with the oleic acid light one-level.In addition, the oleic acid that uses is in an embodiment supplied with the stainless steel sift (ア ズ ワ Application company system) of sieve aperture 25 μ m in order to remove contained impurity.Utilize this operation, can prevent the obstruction in the various holes such as hole of separatory membrane 24.
In addition, the ratio of mixture of oleic acid and methanol solution is 7.18:1, in order to react more quickly excessive use methyl alcohol.To the liquor charging flow that mixes with microreactor 3 oleic acid is made as 0.898ml/ minute, methanol solution is set as 0.125ml/ minute.That is, to set pump 2a, 2b to the total liquor charging flow that mixes the raw material of supplying with microreactor 3 as 1.023ml/ minute mode.
The liquor charging of raw material uses the little processing server MPS-α of microreactor system of Hitachi 200 (Hitachi Plant Technologies company system).MPS-α 200 is the systems with the syringe pump liquor charging, when liquor charging, program liquor charging pattern with MPS-α 200, by two syringe pumps (being equivalent to pump 2a, 2b) alternately being aspirated repeatedly and/or spue, use in the mode of the liquid of the volume more than the capacity that can send incessantly syringe pump.
As mixing with microreactor 3, use the microreactor CMPS-processed α of Hitachi Plant Technologies company 04.
In addition, carry out section 4 as chemical time, use the fluororesin tube (GL サ イ エ Application ス company system) of external diameter 3mm, internal diameter 2mm, long 10m.
Moisture with structure shown in Figure 2 is from be of a size of the structure that contains the T-shaped zeolite membrane (Mitsui shipbuilding society system) as separatory membrane 24 in the inboard of the pipe of internal diameter 16mm with microreactor 6.In addition, moisture is that the diameter of 331mm, the first disc parts 20, the second disc parts 21, flange portion 22a is 40mm from the total length with microreactor 6.The actual measurement of the external diameter of T-shaped zeolite membrane for 12.3mm, longly be 300mm, so the stream of reaction soln stream 25 wide be (1.85mm) below the 2mm.
Influx 20b and reaction soln stream 25 and relief outlet 21e are communicated with, therefore, on the second disc parts 21, along the circumferential direction uniformly-spaced dispose the hole of four diameter 0.2mm.Thus, reaction soln is almost consistent with theoretical value to the flowing time of relief outlet 20e from the influx 20b with microreactor 6 from moisture, utilizes above-mentioned hole, and liquid suitably circulates.
Quantitative use HPLC (the High Performance Liquid Chromatography of resultant (Witconol 2301) and oleic acid residue; High performance liquid chromatography (HPLC)) carries out.
(operating condition)
At first, to add up to 1.023ml/ minute liquor charging flow to use microreactor 3 supply oleic acid and methanol solution as reaction soln to the mixing of immersing 60 ℃ thermostatic bath.Then, make the chemical reaction that 60 ℃ thermostatic bath (that is, the design temperature of temperature adjuster 5 is equivalent to 60 ℃) is immersed in this reaction soln circulation carry out section 4., with identical liquor charging flow to the moisture that immerses 60 ℃ thermostatic bath (that is, the design temperature of temperature adjuster 7 be equivalent to 60 ℃) from usefulness microreactor 6 supply with, in 25 circulations of reaction soln stream thereafter.Then, by utilizing reliever 11 water vapor stream 26 is decompressed to-0.085MPa the water in vaporization and/or the separation of water vapor stream 26.The water that has separated is being reclaimed by ice-cooled cold-trap 10.
After moisture leaves and begins to be set as oleic acid and methanol solution and mix rear 31 minutes.That is, began moisture from using microreactor 6 supply response solution through 31 minutes after the mixing.Then, by after mixing through after 56 minutes, stopped liquor charging 30 minutes, the what is called that begins again afterwards liquor charging " is arrheaed (stopped flow) method ", prolongs the disengaging time of water.
In addition, be attached to the design temperature that mixes with design temperature, temperature adjuster 5 and the temperature adjuster 7 of the temperature adjuster (not shown) of microreactor 3 and all be set as 60 ℃.Although this temperature is lower than the boiling point (64.7 ℃) of methyl alcohol, even very little, also might make the material benzenemethanol gasification, raw material contact area each other reduces, and speed of response slows down.Therefore, control back pressure valve 8 maintains the pressure of reaction system more than the 138kPa (20psi).
(comparative example 1)
Carry out section 4 as chemical reaction, except the fluoro-resin tubulation (GL サ イ エ Application ス company system) that uses the about 1.6mm of external diameter, internal diameter 1mm, long 0.1m, study equally with above-described embodiment.In this situation, it is very short that chemical reaction carries out section 4, therefore, uses the reaction soln of microreactor 3 discharges immediately to moisture from supplying with microreactor 6 from mixing.
(comparative example 2)
As a comparative example 2, carry out the research of interrupter method.In the interrupter method, prepare by with T-shaped zeolite membrane cover clamping with silicon rubber up and down, tubular stinger in serum cap thus can be to the device that reduces pressure in the film.In immersing 60 ℃ the round-bottomed flask of 200ml of thermostatic bath, add the oleic acid of 100ml, mix the methanol solution 13.9ml that contains the vitriol oil with the concentration of 1.6 quality % at 1 minute minute three times while stirring, obtain reaction soln, continue to make while stirring reaction to carry out.
To be made as 20mm with the length of the film of serum cap clamping up and down, this part immerses reaction soln usually, and film is soaked into, and utilizes reliever, by will being decompressed to-0.085MPa the water in vaporization and/or the separation system in the film.The water that has separated is being reclaimed by ice-cooled cold-trap.Carry out 3 hours moisture from, the growing amount of the Witconol 2301 in the assaying reaction solution.
(result)
Fig. 9 represents the coordinate diagram of yield with respect to the elapsed time (that is, chemical time) that begins from mixing.Yield is the yield of the Witconol 2301 of being calculated by following formula (1).
In the formula (1), the volumetric molar concentration of the Witconol 2301 in (Witconol 2301) expression reaction soln, the volumetric molar concentration of the oleic acid in " oleic acid " expression reaction soln.
Shown in Fig. 9 (a), in embodiment 1, before leaving the beginning, moisture reaches equilibrium state with yield 52%.Then, beginning moisture from the time, yield increases, yield is that comparative example 2 is compared abundant raising with existing method.Particularly, yield was 63% when the reaction times was 85 minutes, compared with comparative example 2, increased by 7%.
In addition, shown in Fig. 9 (b) that comparative example is compared each other, be not provided with the identical movement of comparative example 2 demonstration cardinal principles that chemical reaction carries out comparative example 1 and the existing interrupter method of section 4.In addition, though not shown, in comparative example 1, in 55 minutes reaction times, do not observe the separation of water.
In addition, for embodiment 1 and comparative example 1 and 2, calculate the velocity constant k that calculates based on following formula (2)
1, k
-1, k
2(with reference to Fig. 3).The formula of calculating that the below's expression is concrete.
Above result's data are summed up in table 1 expression.
[table 1]
In the table 1, " ※ " expression is not because observing the separation of water, and situation about can not calculate.
From through the moisture after 31 minutes reaction times from situation (embodiment 1), during from the reaction beginning Separation of Water situation (comparative example 1) and can not compare merely but the velocity of separation constant k of water with interrupter method (comparative example 2)
2Compare with comparative example 1, increase by 10
3Times degree, comparing with comparative example 2 increases by 10
8Times degree.So as can be known, use moisture from using microreactor, carry out section 4, expeditiously Separation of Water by chemical reaction further is set.
In addition, in the situation of embodiment 1, the velocity constant k of the positive reaction of (before namely 31 minutes) before the separation of water begins
1Larger than comparative example 1 and comparative example 2.Therefore, carry out section 4 by chemical reaction is set as can be known, can shorten chemical time.
According to above result as can be known, according to present embodiment, can high efficiency separation water, obtain high yield with short chemical time simultaneously.
Claims (6)
1. water separating system separates its resultant solution that water is obtained after making the raw material chemical reaction, it is characterized in that possessing:
Mixing device, described mixing device is supplied with described raw material and is mixed;
Chemical reaction carries out device, and described chemical reaction carries out the downstream that device is connected in described mixing device, carries out the chemical reaction of the described raw material through mixing;
Water separation device, described water separation device is connected in the downstream that described chemical reaction carries out device, is separated in described chemical reaction and carries out the water that generates in the device; And
Control device, described control device is controlled the chemical time that described chemical reaction carries out device,
Described control device carries out following control:
When the amount of the resultant carry out the solution that device discharges from described chemical reaction is many, shortens described chemical reaction and carry out chemical time in the device,
When the amount of the resultant carry out the solution that device discharges from described chemical reaction is few, prolongs described chemical reaction and carry out chemical time in the device.
2. water separating system as claimed in claim 1 is characterized in that,
Described control device possesses control to the function of the liquor charging flow of the raw material of described mixing device supply,
By the liquor charging flow of control to the raw material of described mixing device supply, control chemical time.
3. water separating system as claimed in claim 1 is characterized in that,
Described chemical reaction carries out device and has fine channel,
By changing the length of described fine channel, the control chemical time.
4. water separating system as claimed in claim 3 is characterized in that,
Described chemical reaction carries out device and is made of the equipment of the fine channel with specified length,
By being connected in series one or more described equipment, set the length of described fine channel.
5. such as each described water separating system in the claim 1～4, it is characterized in that possessing:
The chemical reaction temperature control device, the temperature during described chemical reaction temperature control device control chemical reaction; And
Moisture is from temperature-control device, described moisture from temperature-control device control moisture from the time temperature;
Temperature during with chemical reaction and moisture from the time Temperature Setting be different.
6. such as each described water separating system in the claim 1～5, it is characterized in that,
Be provided with the on-line determination device of the amount of measuring described resultant.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011163395A JP5452552B2 (en) | 2011-07-26 | 2011-07-26 | Water separation system |
| JP2011-163395 | 2011-07-26 |
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| CN102898302A true CN102898302A (en) | 2013-01-30 |
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| CN201210242576XA Pending CN102898302A (en) | 2011-07-26 | 2012-07-13 | Water separating system |
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| JP (1) | JP5452552B2 (en) |
| CN (1) | CN102898302A (en) |
| DE (1) | DE102012213103A1 (en) |
| FR (1) | FR2978359A1 (en) |
| SG (1) | SG187365A1 (en) |
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| JP6924556B2 (en) | 2016-04-12 | 2021-08-25 | 株式会社日立プラントサービス | Microreactor, chemical product manufacturing system and microreactor manufacturing method |
| CN110655460A (en) * | 2018-06-29 | 2020-01-07 | 江苏紫奇化工科技有限公司 | Method for continuously synthesizing isooctyl salicylate in micro-channel |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5248427A (en) * | 1990-09-15 | 1993-09-28 | Basf Aktiengesellschaft | Removal of water from mixtures with alcohols and/or carboxylic acids and/or carboxylic esters |
| US5976324A (en) * | 1996-10-14 | 1999-11-02 | Bayer Aktiengesellschaft | Removal of water from reaction mixtures |
| US20030068790A1 (en) * | 1997-02-14 | 2003-04-10 | Van Gemert Robert Wilhelm | Enzymatically catalysed process |
| CN201454511U (en) * | 2009-07-03 | 2010-05-12 | 中国石油天然气股份有限公司 | Pervaporation-reaction coupling device for preparing dimethyl adipate |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH093003A (en) * | 1995-06-22 | 1997-01-07 | Mitsubishi Chem Corp | Production of plasticizer |
| JP2002047213A (en) * | 2000-08-03 | 2002-02-12 | Mitsui Eng & Shipbuild Co Ltd | Apparatus for esterifying reaction and method for producing ester using the same |
| JP4560605B2 (en) * | 2003-01-15 | 2010-10-13 | 独立行政法人産業技術総合研究所 | Chemical reaction control method |
| JP4462884B2 (en) * | 2003-09-25 | 2010-05-12 | 三井造船株式会社 | Membrane separation reaction system |
| KR20050037240A (en) * | 2003-10-17 | 2005-04-21 | 한국화학연구원 | New esterfication process for production of fluoroalkyl (meth)acrylate by pervaporation-aided membrane reactor |
| JP2007203210A (en) | 2006-02-02 | 2007-08-16 | Mitsui Eng & Shipbuild Co Ltd | Membrane module and membrane separation process |
-
2011
- 2011-07-26 JP JP2011163395A patent/JP5452552B2/en active Active
-
2012
- 2012-07-13 CN CN201210242576XA patent/CN102898302A/en active Pending
- 2012-07-25 DE DE201210213103 patent/DE102012213103A1/en not_active Ceased
- 2012-07-25 FR FR1257230A patent/FR2978359A1/en not_active Withdrawn
- 2012-07-26 SG SG2012055570A patent/SG187365A1/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5248427A (en) * | 1990-09-15 | 1993-09-28 | Basf Aktiengesellschaft | Removal of water from mixtures with alcohols and/or carboxylic acids and/or carboxylic esters |
| US5976324A (en) * | 1996-10-14 | 1999-11-02 | Bayer Aktiengesellschaft | Removal of water from reaction mixtures |
| US20030068790A1 (en) * | 1997-02-14 | 2003-04-10 | Van Gemert Robert Wilhelm | Enzymatically catalysed process |
| CN201454511U (en) * | 2009-07-03 | 2010-05-12 | 中国石油天然气股份有限公司 | Pervaporation-reaction coupling device for preparing dimethyl adipate |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2978359A1 (en) | 2013-02-01 |
| SG187365A1 (en) | 2013-02-28 |
| DE102012213103A1 (en) | 2013-01-31 |
| JP5452552B2 (en) | 2014-03-26 |
| JP2013027798A (en) | 2013-02-07 |
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