CN105797661A - Reaction device, and vanillin production equipment and production method - Google Patents
Reaction device, and vanillin production equipment and production method Download PDFInfo
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- CN105797661A CN105797661A CN201410854887.0A CN201410854887A CN105797661A CN 105797661 A CN105797661 A CN 105797661A CN 201410854887 A CN201410854887 A CN 201410854887A CN 105797661 A CN105797661 A CN 105797661A
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Abstract
The invention discloses a reaction device used for condensation reaction of glyoxylic acid and guaiacol, vanillin production equipment containing the reaction device, and a vanillin production method. The reaction device used for condensation reaction of glyoxylic acid and guaiacol provided by the invention comprises a reaction tower set with a total liquid inlet and a total liquid outlet, wherein the reaction tower set comprises at least one vertically-arranged reaction tower; the lower part of the reaction tower is provided with a liquid inlet, and the upper part of the reaction tower is provided with a liquid outlet; the liquid inlet communicates with the total liquid inlet, and the liquid outlet communicates with the total liquid outlet; at least one sieve plate with through-flow holes is arranged inside the reaction tower; and at least one part of the surface of the sieve plate is not parallel with the center line of the reaction tower. The vanillin production equipment disclosed by the invention comprises the reaction device, and the vanillin production method disclosed by the invention adopts the above-mentioned vanillin production equipment. By utilizing the above-mentioned reaction device, conversion rate and selectivity of condensation reaction can be guaranteed, and industrial operation cost is reduced at the same time.
Description
Technical field
The present invention relates to and produce chemical synthesising technology for vanillin, particularly to a kind of reaction unit for glyoxalic acid and guaiacol condensation, and the vanillin including this reaction unit produces equipment and vanillin production method.
Background technology
Vanillin is the fixastive of a kind of food additive, essence, is widely used in the preparation of Nicotiana tabacum L. and all kinds of cosmetic essence.
At present, commercial synthesis is the main mode obtaining vanillin.Commercial synthesis mode mainly has Nitrosation Process and acetaldehyde acid system.Acetaldehyde acid system includes the courses of reaction such as condensation, neutralization, wood phenol extraction, oxidation, decarboxylation.Wherein, condensation reaction is important course of reaction, in this course of reaction, the reactant liquor including glyoxalic acid and guaiacol (formal name used at school o-methoxyphenol) reacts in suitable reaction unit, converts and prepared principal product mandelic acid (3 methoxy 4 hydroxymandelic acid).In condensation reaction, conversion ratio and selectivity are the important parameters characterizing condensation reaction effect.More complicated based on glyoxalic acid and guaiacol condensation reaction, including primary response (desired reaction) and side reaction (less desirable reaction).Side reaction carries out more few, and the selectivity of glyoxalic acid is more high；Therefore, in the condensation reaction, control reaction process and become the key of condensation reaction.
In the field of business, the reaction unit that condensation reaction adopts is generally stirred-tank reactor.More complicated based on glyoxalic acid and guaiacol condensation reaction, including primary response (desired reaction) and side reaction (less desirable reaction).When utilizing stirred-tank reactor to carry out condensation reaction, industrial very difficult control still reacts, and then affects the selectivity of condensation reaction；It addition, stirred-tank reactor also needs to arrange the agitating device consuming power, operating cost is higher.A kind of technology utilizing tubular reactor to carry out condensation reaction disclosed in Chinese patent literature CN101835734B; but utilize this technology to need reactant liquor to have higher Reynolds number or at reaction unit with filler; in order to ensure that condensation reaction comparatively fast carries out; needing higher temperature in industrial course of reaction and arrange catalyst and noble gas is protected, this makes the industrial operating cost can be significantly high.
Therefore, how ensureing conversion ratio and be selective while, reducing industry park plan cost is the technical barrier that people in the art to solve.
Summary of the invention
Based on above-mentioned technical barrier, the purpose of a first aspect of the present invention is in that to provide a kind of reaction unit for glyoxalic acid and guaiacol condensation, utilizes this reaction unit ensureing condensation reaction transformation ratio and be selective while, can reduce industry park plan cost.
The purpose of a second aspect of the present invention is in that to provide a kind of vanillin including above-mentioned reaction unit produce equipment and utilize the production method of this production equipment, to ensure conversion ratio and the selectivity of production process Raw, reduces industry park plan cost.
In reaction unit for glyoxalic acid and guaiacol condensation provided by the invention, including the reaction tower system with total inlet and total liquid outlet, described reaction tower system at least includes a vertically arranged reaction tower, forms reaction compartment in reaction tower；Described reaction tower bottom arranges inlet, and top is provided with liquid outlet, and described flow inlet connects with described total inlet, and described liquid outlet connects with described total liquid outlet；Reactant liquor thus can be made to enter reaction tower system from total inlet, and carry out condensation by the reaction compartment in corresponding inlet entrance reaction tower, and flow out respective reaction tower (or flowing out reaction tower system from total liquid outlet) by liquid outlet.Meanwhile, at least provided with a sieve plate being provided with through flow hole in described reaction tower；At least some of surface of described sieve plate is not parallel with the centrage of described reaction tower, and so, sieve plate just can form the resistance to reactant liquor flowing, makes the reactant liquor before sieve plate carry out back mixing, and then makes reactant liquor reduce in the time of staying difference of reaction tower；Through flow hole on sieve plate can make back mixing after reactant liquor flow up smoothly, ensure reactant liquor entirety flow forward, reducing the back mixing between the reactant liquor before and after sieve plate, the side reaction reducing reactant liquor on the whole occurs, it is ensured that the conversion ratio of condensation reaction and selectivity；Utilize this reaction unit simultaneously, the rabbling mechanism consuming power need not be set, reactant liquor can be made with relatively low speed flowing (laminar condition), and then condensation reaction time can be extended, basis is provided, it is possible to reduce industry park plan cost for carrying out condensation reaction under low temperature, catalyst-free state.
In further technical scheme, described sieve plate is positioned at the center of described reaction tower, and has distance between the inwall of sieve plate periphery and described reaction tower.So can increase the resistance of reactant liquor center, make reactant liquor near core reactant liquor and inwall reduce in reaction tower time of staying difference.In order to manufacture with easy for installation, in further technical scheme, it is possible to make the periphery of sieve plate coordinate with the inwall of described reaction tower；The central axis of described sieve plate and described reaction tower can also be made；Sieve plate can be surface plate.In order to reduce the laminar flow adverse effect to the time of staying, can also at least provided with the described sieve plate being evenly arranged on 6 above-below directions in reaction tower, space in described reaction tower is divided at least 7 parts, to form the other back mixing of more stages, the side reaction reducing reactant liquor on the whole occurs, it is ensured that the conversion ratio of condensation reaction and selectivity.
In further technical scheme, described reaction tower system includes the reaction tower of multiple order series winding, and the head piece that goes out of previous described reaction tower connects with the flow inlet of reaction tower described in later；The inlet of the most forward reaction tower is connected with described total inlet, and the liquid outlet of described described reaction tower the most rearward is connected with described total liquid outlet.So can increase the general reaction space of reaction unit, facilitate setting and the layout of reaction tower, reduce plant area's equipment cost.
In further technical scheme, reaction unit also includes condensation heat-exchanger rig；Described condensation heat-exchanger rig includes the first heat exchanger, and described first heat exchanger has condensation liquid passage and proportion liquid passage；Described total liquid outlet is connected with the import of described condensation liquid passage.Make reactant liquor pass through condensation liquid passage, make dispensing liquid by proportion liquid passage, condensation liquid and dispensing liquid so can be made to carry out heat exchange, comprehensively utilize energy, provide basis for reducing industry park plan cost.
In further technical scheme, described condensation heat-exchanger rig also includes the second heat exchanger；Described reactant liquor passage described second heat exchanger of traverse；Described second heat exchanger also includes the 3rd medium cooling duct.Same principle, it is possible to so that condensation liquid and other liquid carry out heat exchange, comprehensively utilize energy, provides basis for reducing industry park plan cost.
In further technical scheme, reaction unit also includes at least one heat exchange reaction tower, and described heat exchange reaction tower bottom arranges inlet, and top is provided with liquid outlet；The outlet of described reactant liquor passage is connected with the inlet of described heat exchange reaction tower.So, heat exchange reaction tower can just be entered by the reactant liquor of condensation heat-exchanger rig；Raised by the reacting liquid temperature after condensation heat-exchanger rig, it is possible to promote condensation reaction, and then be conducive to glyoxalic acid (sodiam glyoxlate) to react completely, improve the conversion ratio of glyoxalic acid.
The vanillin provided produces equipment and includes glyoxalic acid proportioner, wood phenol proportioner and condensation feed arrangement, also the liquid outlet of any of the above-described kind of reaction unit for glyoxalic acid and guaiacol condensation, the liquid outlet of described glyoxalic acid proportioner and wood phenol proportioner is connected with the inlet of described condensation feed arrangement respectively；The liquid outlet of described condensation feed arrangement is connected with described total inlet.Owing to having above-mentioned reaction unit, this vanillin produces equipment and also has corresponding technique effect.
The vanillin production method provided, utilizes above-mentioned vanillin to produce equipment, and the method includes condensation reaction, and this condensation reaction includes: obtain sodiam glyoxlate solution by described glyoxalic acid proportioner, obtains sodium phenolate solution by described wood phenol proportioner；Make sodiam glyoxlate solution and phenol sodium liquid be mixed to form reactant liquor by condensation feed arrangement and enter total inlet of described reaction tower system, by described reaction tower, and discharge from total liquid outlet of described reaction tower system after at least keeping 16 hours in described reaction tower system；In described reaction tower, the temperature of described reactant liquor is maintained between 13-30 degree, and flowing velocity is between 0.010m/s-0.0030m/s.Utilize the method; owing to reaction temperature is relatively low; and the time of staying is longer, reactant liquor flowing velocity in reaction tower is relatively low, and Reynolds number (Reynolds number is directly proportional to reactant liquor flowing velocity) is relatively low; catalyst need not be set in reaction compartment; protect also without arranging noble gas in reaction compartment, it is not required that the agitating device consuming power is set and is stirred, and then; ensureing condensation reaction transformation ratio and be selective while, industry park plan cost can be reduced.
In further technical scheme, the reactant liquor discharged from total liquid outlet of described reaction tower system is made to pass through reactant liquor passage, dispensing liquid is made to be flowed to described glyoxalic acid proportioner and/or the predetermined proportion liquid mouth of wood phenol proportioner by described proportion liquid passage, from the temperature rising of the reactant liquor that total liquid outlet of described reaction tower system is discharged, dispensing temperature of liquid reduces；Reactant liquor after elevating the temperature enters the reaction chamber of described heat exchange reaction tower by the inlet of described heat exchange reaction tower, then discharges from the inlet of described heat exchange reaction tower；In described heat exchange reaction tower, the temperature of reactant liquor is maintained at 38-50 degree.The temperature of reactant liquor can be made to improve on the one hand, reactant liquor proceeds condensation reaction after entering heat exchange reaction tower, higher temperature can improve the conversion ratio of glyoxalic acid, and such condensation reaction just includes the low-temp reaction in reaction tower system and the pyroreaction in heat exchange reaction tower；Condensation reaction is divided into two stages can while ensureing conversion ratio, it is ensured that or improve selectivity, and meanwhile, reducing heat supply needs；On the other hand, it is possible to reduce dispensing temperature of liquid, owing to the setting-up point temperature in reaction tower system is relatively low, it is possible to reduce the cooling power demand to dispensing liquid.And then vanillin production industry park plan cost can be reduced both ways.
Accompanying drawing explanation
The accompanying drawing constituting the part of the present invention is used for providing a further understanding of the present invention, and the schematic description and description of the present invention is used for explaining the present invention, is not intended that inappropriate limitation of the present invention.
Fig. 1 produces the structural representation of equipment for a kind of vanillin that the embodiment of the present invention one provides；
Fig. 2 produces the structural representation of equipment for a kind of vanillin that the embodiment of the present invention two provides；
In the vanillin production equipment that Fig. 3 provides for embodiment three, the part-structure schematic diagram of reaction tower；
Fig. 4 is A-A sectional structure chart in Fig. 2；
Fig. 5 is the sieve plate schematic diagram of a kind of cone-plate structure.
In figure:
Glyoxalic acid proportioner 100；Wood phenol proportioner 200；Condensation feed arrangement 300；Reaction unit 400；Reaction tower system 410；Reaction tower 411；Sieve plate 401；Condensation heat-exchanger rig 420；First heat exchanger 421；Second heat exchanger 422；Heat exchange reaction tower 430.
Detailed description of the invention
Hereinafter example provided by the invention is described in detail.It should be noted that when not conflicting, the example in the present invention and the feature in example can be mutually combined.For the ease of understanding, in this part, while the vanillin that present example is provided produces equipment, the reaction unit for glyoxalic acid and guaiacol condensation that present example is provided is described, and no longer the reaction unit for glyoxalic acid and guaiacol condensation is individually described.It is to be understood that, the reaction unit for glyoxalic acid and guaiacol condensation can be carried out as independent technical scheme, it is possible to produces other relevant devices of equipment with vanillin and is incorporated into the production of row vanillin.
Ratio in presents, between molal quantity that conversion ratio refers to the glyoxalic acid being converted and the molal quantity of glyoxalic acid joined in reaction unit.Ratio between molal quantity that selectivity refers to the mandelic acid of acquisition and the molal quantity of glyoxalic acid being converted.
Describe the present invention in detail below with reference to the accompanying drawings and in conjunction with example.
Refer to Fig. 1, this figure is the structural representation that a kind of vanillin that present example one provides produces equipment.This vanillin produces equipment and includes glyoxalic acid proportioner 100, wood phenol proportioner 200 and condensation feed arrangement 300, also includes this reaction unit 400 for glyoxalic acid and guaiacol condensation.Reaction unit 400 includes the reaction tower system 410 (in Fig. 1 part in broken box) with total inlet and total liquid outlet.
In the present embodiment, glyoxalic acid proportioner 100 is used for obtaining sodiam glyoxlate solution；Glyoxalic acid proportioner 100 specifically can include glyoxalic acid batching kettle.Sodiam glyoxlate solution is obtained by mixing glyoxalic acid, liquid caustic soda and water.Wood phenol proportioner 200 is used for obtaining sodium phenolate solution；Wood phenol proportioner 200 specifically can include wood phenol batching kettle, obtains sodium phenolate solution by mixing guaiacol, liquid caustic soda and water.Condensation feed arrangement 300 can be feed pump.Certainly, predetermined reaction raw materials can be obtained according to concrete reaction needed, glyoxalic acid proportioner 100 and wood phenol proportioner 200.Certainly, before sodiam glyoxlate solution and sodium phenolate solution enter condensation feed arrangement 300, it is also possible to condensation kettle is set, after making sodiam glyoxlate solution and sodium phenolate solution mixing, condensation feed arrangement 300 is entered back into.
In the present embodiment, reaction tower system 410 includes 7 vertically arranged reaction towers 411, forms predetermined reaction compartment in each reaction tower 411.In the present embodiment, 7 reaction tower 411 order series windings, each reaction tower 411 bottom arranges inlet, and top is provided with liquid outlet.With reactant liquor flow direction for reference, after flow direction is, rightabout is front.The head piece that goes out of previous reaction tower 411 connects with the flow inlet of later reaction tower 411；The inlet of the most forward reaction tower 411 is connected with total inlet, and the liquid outlet of reaction tower 411 the most rearward is connected with total liquid outlet.So can increase the general reaction space of reaction unit, the convenient setting reacting tower system 410 and layout, reduce plant area's equipment cost.In the present embodiment, the height of each reaction tower 411 is 20 meters, and diameter is 2 meters, and the overall reaction space of 7 reaction tower series winding formation is approximately 480 cubic metres.Certainly, according to actual needs, it is possible to one or more reaction tower 411 is set；The concrete size of reaction tower 411 can also need to be adjusted according to actual industrial production.
Refer to Fig. 1, each reaction tower 411 arranges multiple sieve plate 401 with through flow hole.In the present embodiment, sieve plate 401 is circular flat panel, and periphery coordinates with the inwall of corresponding reaction tower 411, it is possible to be fixed on the inwall of reaction tower 411；The central axis of sieve plate 401 extended planar and reaction tower 411.In the present embodiment, being provided with 6 sieve plates being uniformly arranged in the vertical direction 401 in each reaction tower 411, namely 6 sieve plate upper and lower upstream sequences are arranged, the reaction compartment in each reaction tower 411 is divided into 7 of substantially equal parts.In the present embodiment, the through flow hole on sieve plate 401 is equal in magnitude, is diameter 50mm, and is evenly arranged on sieve plate 401 surface.It is appreciated that according to factors such as condensation reaction needs and reactant liquor viscosity different, it is possible to so that through flow hole is arranged with predetermined rule on sieve plate 401 surface, make diverse location have different flow area；It is of course also possible to according to reaction tower 411 height and reaction needed, reaction tower 411 arranges one or more sieve plate 401.
As shown in the figure, reactant liquor can enter reaction tower system 410 from total inlet, and carry out condensation by the reaction compartment in the corresponding inlet each reaction tower 411 of entrance, and by liquid outlet stream to next reaction tower 411, flow out reaction tower system 410 finally by total liquid outlet.When reactant liquor is by respective reaction tower 411, sieve plate 401 can form the resistance to reactant liquor flowing, makes the reactant liquor before sieve plate 401 carry out back mixing, and then makes reactant liquor reduce in the time of staying difference of reaction tower 411；Through flow hole on sieve plate 401 can make back mixing after reactant liquor flow up smoothly, ensure reactant liquor entirety flow forward, reducing the back mixing between the reactant liquor before and after sieve plate 401, the side reaction reducing reactant liquor on the whole occurs, it is ensured that the conversion ratio of condensation reaction and selectivity.
Should be noted that: without sieve plate 401, reactant liquor is when reaction tower 411 flows, and its particle is along for linear motion with the direction of reaction tower 411 centerline parallel, and the flow velocity of reactant liquor is maximum in the centerline of reaction tower 411, minimum near inwall place, for " laminar condition "；Under layer liquid status, the core of reaction tower 411 is very big with the reactant liquor of inner wall section time of staying difference in reaction tower；Sieve plate 401 can make reactant liquor reduce in the time of staying difference of reaction tower 411.Certainly, it can also be the part of reaction tower 411 horizontal cross-section that sieve plate 401 projects in a vertical direction, as long as the centrage of at least some of surface of sieve plate 401 and reaction tower 411 not parallel (namely with the central axis of reaction tower 411 or shape in an angle), just can form the resistance to reactant liquor flowing, produce the effect above.Maximum in the centerline of reaction tower based on the flow velocity of reactant liquor under " laminar condition ", therefore, sieve plate 401 can be made to be positioned at the center of reaction tower 411, and can make, between the inwall of sieve plate 401 periphery and respective reaction tower 411, there is distance, to reduce the flow resistance of the reactant liquor near inwall.
Utilize this reaction unit 400, owing to the rabbling mechanism consuming power need not be arranged, reactant liquor can be made with relatively low speed flowing (laminar condition), and then condensation reaction time can be extended, basis is provided, it is possible to reduce industry park plan cost for carrying out condensation reaction under low temperature, catalyst-free state.
In the present embodiment, reaction unit 400 also includes condensation heat-exchanger rig 420；Condensation heat-exchanger rig 420 includes the first heat exchanger 421, and the first heat exchanger 421 has reactant liquor passage and proportion liquid passage；Total liquid outlet of reaction tower system 410 is connected with the import of reactant liquor passage.In the present embodiment, namely the liquid outlet of last reaction tower 411 is connected with the import of reactant liquor passage.The reactant liquor after condensation so can be made in reaction tower system by reactant liquor passage；Simultaneously, it is possible to make dispensing liquid (such as, forming the water required for reaction raw materials) by proportion liquid passage；And then make reactant liquor and dispensing liquid carry out heat exchange, comprehensively utilize energy, provide basis for reducing industry park plan cost.
As it is shown in figure 1, in the present embodiment, it is possible to make the reactant liquor that the total liquid outlet from reaction tower system 410 is discharged by reactant liquor passage, make dispensing water be flowed to the filler of glyoxalic acid proportioner 100 and the filler of wood phenol proportioner 200 by proportion liquid passage.Of course, it is possible to make dispensing liquid individually flow to the filler of glyoxalic acid proportioner 100 or the filler of wood phenol proportioner 200.
It addition, in the present embodiment, condensation heat-exchanger rig 420 also includes the second heat exchanger 422；Reactant liquor passage again passes through the second heat exchanger 422；Second heat exchanger 422 also includes the 3rd medium cooling duct.Same principle so that it is he passes through the 3rd medium cooling duct by liquid, it is possible to so that condensation liquid and other liquid carry out heat exchange, comprehensively utilize energy, provides basic for reducing industry park plan cost.
In the vanillin production method embodiment provided, the vanillin that above-described embodiment one provides just is utilized to produce equipment.In the method, condensation reaction specifically includes:
Obtain sodiam glyoxlate solution by glyoxalic acid proportioner 100, obtain sodium phenolate solution by wood phenol proportioner 200.And make the substantially 0.7:1 to 0.8:1 of the mol ratio between main material glyoxalic acid and guaiacol.
Make sodiam glyoxlate solution and phenol sodium liquid be mixed to form reactant liquor by condensation feed arrangement 300 and enter total inlet of described reaction tower system 410, order is by each reaction tower 411, and discharges from total liquid outlet of reaction tower system 410 after at least keeping the scheduled time in reaction tower system 410；In each reaction tower 411, the temperature of reactant liquor is maintained in predetermined scope, and is controlled between predetermined scope by the Reynolds number of the flowing velocity of reactant liquor.
Utilize the tables of data that above-mentioned vanillin production equipment and production method carry out producing as follows:
In above table, the reactant liquor time of staying in reaction tower system can be passed through to change reactant liquor feed speed (or flowing velocity that reactant liquor is in reaction tower) and is adjusted: as made reactant liquor feed speed substantially keep 40m3/ s, makes reactant liquor flow velocity in reaction tower substantially keep 0.1118m/s, it is possible to make reactant liquor time of staying in reaction tower substantially remain in 24 hours.
According to above-mentioned data, in the condensation reaction, will reaching high selectivity, depend primarily on temperature control, if temperature improves 8-10 degree, selectivity will decline 5%；And to reach high conversion, reactant liquor will be made as much as possible to stop the longer time (such as 24 hours) at reaction tower system 410.
Owing to the 70-80% of the cost of vanillin production is the cost of raw material, it is therefore preferable that produce vanillin when reaction tower interior reaction temperature 15-18 degree.Therefore, utilizing said method, owing to reaction temperature is relatively low, and the time of staying is longer, and reactant liquor flowing velocity in reaction tower 411 is relatively low, and Reynolds number is relatively low；Catalyst need not be set in the reaction compartment of reaction tower 411, it is not necessary to noble gas is set in reaction compartment and protects, it is not required that the agitating device consuming power is set and is stirred.According to measuring and calculating, owing to need not arrange agitating device, vanillin per ton reduces electric power consumption 960KWH.
Utilizing said method, when producing vanillin when reaction tower interior reaction temperature 15-18 degree, dispensing water is made to be flowed to glyoxalic acid proportioner 100 and the filler of wood phenol proportioner 200 by proportion liquid passage, such that it is able to make the reacting liquid temperature that total liquid outlet of reaction tower system 410 is discharged raise, dispensing coolant-temperature gage reduces.So, making the reacting liquid temperature by reacting tower system improve on the one hand, it is possible to provide good condition for subsequent reactions, reducing heat supply needs；Through measuring and calculating, so can save and add vapours 800KG/T vanillin.On the other hand, it is possible to reduce dispensing liquid temperature, due in reaction tower setting-up point lower than room temperature, it is possible to reduce the cooling power demand to dispensing liquid；According to measuring and calculating, refrigerating capacity 9.5 × 10 so can be saved4KJ/T。
And then, adopt above-mentioned production equipment and production method ensureing condensation reaction transformation ratio and be selective while, industry park plan cost can be reduced.
The embodiment of the present invention two provides another kind of vanillin to produce equipment.If Fig. 2, this figure are the structural representations that a kind of vanillin that the embodiment of the present invention two provides produces equipment.Compared with producing equipment with the vanillin that embodiment one provides, in the vanillin production equipment that embodiment two provides, reaction unit 400 also includes a heat exchange reaction tower 430.Identical with above-mentioned reaction tower 411, the bottom of this heat exchange reaction tower 430 arranges inlet, and top is provided with liquid outlet；In the present embodiment, the overall dimensions of this heat exchange reaction tower 430 and reaction tower 411 equivalently-sized, the two is distinctive in that, is not provided with sieve plate in heat exchange reaction tower 430.And, the outlet of the reactant liquor passage of condensation heat-exchanger rig 420 is connected with the inlet of this heat exchange reaction tower 430.
When adopting the vanillin production method that the vanillin that embodiment two provides produces equipment and above-described embodiment offer, reactant liquor is improved by temperature after the reactant liquor passage of condensation heat-exchanger rig 420, reactant liquor after can elevating the temperature enters the reaction chamber of described heat exchange reaction tower by the inlet of described heat exchange reaction tower 430, then discharge from the inlet of heat exchange reaction tower 430, and in described heat exchange reaction tower 430, make the temperature of reactant liquor be maintained at 38-50 degree.
Utilize the vanillin that embodiment two provides to produce equipment, it is thus achieved that creation data as follows:
According to above-mentioned data, it may be determined that when reactant liquor passes through the reaction chamber of heat exchange reaction tower 430, higher temperature can improve the conversion ratio of glyoxalic acid.Such condensation reaction just includes the low-temp reaction in reaction tower system and the pyroreaction in heat exchange reaction tower；Condensation reaction is divided into two stages can while ensureing conversion ratio, it is ensured that or improve selectivity.It is appreciated that the reaction temperature in heat exchange reaction tower 430 can control within certain scope, as can between 38 degree to 50 degree；As being 42 degree, 45 degree or 47 degree.
It is appreciated that heat exchange reaction tower 430 can also be identical with the structure of reaction tower 411, the heat exchange reaction tower 430 of multiple series winding can also be set as required.
The embodiment of the present invention three provides another kind of vanillin and produces equipment.As in the vanillin production equipment that Fig. 3 and Fig. 4, Fig. 3 provide for embodiment three, the part-structure schematic diagram of reaction tower；Fig. 4 is A-A sectional structure chart in Fig. 3.Compared with producing equipment with the vanillin that embodiment two provides, the vanillin that embodiment three provides produces equipment and is distinctive in that: sieve plate 401 size is different, therefore, only describes its difference part below.
In embodiment three, reaction tower diameter remains as 2 meters, but sieve plate 401 is the circular flat board that diameter is 1.2 meters, and is evenly arranged through flow hole on this sieve plate 401.Sieve plate 401 is centrally located on the centrage of reaction tower 411, has the distance of 0.4 meter between the internal face of periphery and reaction tower 411.
When adopting the vanillin that embodiment three provides to produce the vanillin production method that equipment and above-described embodiment provide, it is thus achieved that creation data as follows:
Above-mentioned data illustrate, the time of staying concordance of reactant liquor may be produced certain impact by sieve plate 401, and then conversion ratio has certain impact, but adopts this sieve plate 401 still can realize the goal of the invention of the present invention.
According to foregoing description, it will be understood that sieve plate 401 is not limited to surface plate, it is also possible to be the sieve plate of another kind of pyramidal structure as shown in Figure 5；Certainly, can also according to reaction liquid characteristic and reaction needed, sieve plate 401 is set to curved slab, corrugated sheet etc., drag effect is produced with the reactant liquor to relevant position, reactant liquor is carried out water conservancy diversion simultaneously, control the flowing of reactant liquor, the concordance of reactant liquor time of staying in reaction tower 411 is affected.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (15)
1. the reaction unit for glyoxalic acid and guaiacol condensation, it is characterized in that, including the reaction tower system (410) with total inlet and total liquid outlet, described reaction tower system (410) at least includes a vertically arranged reaction tower (411)；Described reaction tower (411) bottom arranges inlet, and top is provided with liquid outlet；Described flow inlet connects with described total inlet, and described liquid outlet connects with described total liquid outlet；
At least provided with a sieve plate (401) with through flow hole in described reaction tower (411)；At least some of surface of described sieve plate (401) is not parallel with the centrage of described reaction tower (411).
2. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 1, it is characterized in that, described sieve plate (401) is positioned at the center of described reaction tower (411), and has distance between the inwall of described sieve plate (401) periphery and described reaction tower (411).
3. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 1, it is characterised in that the periphery of described sieve plate (401) coordinates with the inwall of described reaction tower (411).
4. the reaction unit for glyoxalic acid and guaiacol condensation according to any one of claim 1-3, it is characterised in that described sieve plate (401) is surface plate.
5. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 4, it is characterised in that the central axis of described sieve plate (401) and described reaction tower (411).
6. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 5, it is characterized in that, at least provided with the described sieve plate (401) being evenly arranged on 6 above-below directions in described reaction tower (411), described reaction tower (411) interior space is divided at least 7 parts.
7. the reaction unit for glyoxalic acid and guaiacol condensation according to any one of claim 1-3, it is characterized in that, described reaction tower system (410) includes the reaction tower (411) of multiple order series winding, and the head piece that goes out of previous described reaction tower (411) connects with the flow inlet of reaction tower described in later (411)；The inlet of the most forward reaction tower (411) is connected with described total inlet, and the liquid outlet of described described reaction tower (411) the most rearward is connected with described total liquid outlet.
8. the reaction unit for glyoxalic acid and guaiacol condensation according to any one of claim 1-3, it is characterised in that also include condensation heat-exchanger rig (420)；Described condensation heat-exchanger rig (420) includes the first heat exchanger (421), and described first heat exchanger (421) has condensation liquid passage and proportion liquid passage；Described total liquid outlet is connected with the import of described condensation liquid passage.
9. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 8, it is characterised in that described condensation heat-exchanger rig (420) also includes the second heat exchanger (422)；Described condensation liquid passage described second heat exchanger (422) of traverse；Described second heat exchanger (422) also includes the 3rd medium cooling duct.
10. the reaction unit for glyoxalic acid and guaiacol condensation according to claim 8, it is characterized in that, also including at least one heat exchange reaction tower (430), described heat exchange reaction tower (430) bottom arranges inlet, and top is provided with liquid outlet；The outlet of described reactant liquor passage is connected with the inlet of described heat exchange reaction tower (430).
11. a vanillin produces equipment, including glyoxalic acid proportioner (100), wood phenol proportioner (200) and condensation feed arrangement (300), it is characterized in that, the liquid outlet also including the reaction unit for glyoxalic acid and guaiacol condensation (400) described in any one of claim 1-7, the liquid outlet of described glyoxalic acid proportioner (100) and wood phenol proportioner (200) is connected with the inlet of described condensation feed arrangement (300) respectively；The liquid outlet of described condensation feed arrangement (300) is connected with described total inlet.
12. vanillin according to claim 10 produces equipment, it is characterised in that also include condensation heat-exchanger rig (420)；Described condensation heat-exchanger rig (420) includes the first heat exchanger (421), and described first heat exchanger (421) has condensation liquid passage and proportion liquid passage；Described total liquid outlet is connected with the import of described condensation liquid passage；The outlet of described proportion liquid passage is connected with the predetermined inlet of glyoxalic acid proportioner (100) and/or wood phenol proportioner (200).
13. vanillin according to claim 12 produces equipment, it is characterised in that also including at least one heat exchange reaction tower (430), described heat exchange reaction tower (430) bottom arranges inlet, and top is provided with liquid outlet；The outlet of described reactant liquor passage is connected with the inlet of described heat exchange reaction tower (430).
14. a vanillin production method, it is characterised in that use the vanillin described in claim 11 to produce equipment；
The method includes condensation reaction, and this condensation reaction includes:
Obtain sodiam glyoxlate solution by described glyoxalic acid proportioner (100), obtain sodium phenolate solution by described wood phenol proportioner (200)；
Make sodiam glyoxlate solution and phenol sodium liquid be mixed to form reactant liquor by condensation feed arrangement (300) and enter total inlet of described reaction tower system (410), by described reaction tower (411), and discharge from total liquid outlet of described reaction tower system (410) after at least keeping 16 hours in described reaction tower system (410)；In described reaction tower (411), the temperature of described reactant liquor is maintained between 13-30 degree, and flowing velocity is between 0.010m/s-0.0030m/s.
15. vanillin production method according to claim 14, it is characterised in that described vanillin produces equipment and also includes condensation heat-exchanger rig (420) and heat exchange reaction tower (430)；Described condensation heat-exchanger rig (420) includes the first heat exchanger (421), and described first heat exchanger (421) has condensation liquid passage and proportion liquid passage；Described total liquid outlet is connected with the import of described condensation liquid passage；The outlet of described proportion liquid passage is connected with the predetermined proportion liquid mouth of described glyoxalic acid proportioner and/or wood phenol proportioner；Described heat exchange reaction tower (430) bottom arranges inlet, and top is provided with liquid outlet；The outlet of described reactant liquor passage is connected with the inlet of described heat exchange reaction tower (430)；
Described condensation reaction also includes:
The reactant liquor discharged from total liquid outlet of described reaction tower system (410) is made to pass through condensation liquid passage, dispensing liquid is made to be flowed to described glyoxalic acid proportioner and/or the predetermined proportion liquid mouth of wood phenol proportioner by described proportion liquid passage, making the temperature rising of the reactant liquor discharged from total liquid outlet of described reaction tower system (410), dispensing temperature of liquid reduces；
Reactant liquor after elevating the temperature enters the reaction chamber of described heat exchange reaction tower by the inlet of described heat exchange reaction tower (430), then discharges from the inlet of described heat exchange reaction tower (430)；In described heat exchange reaction tower (430), the temperature of reactant liquor is maintained at 38-50 degree.
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|---|---|---|---|---|
| US3920750A (en) * | 1974-03-21 | 1975-11-18 | Int Paper Canada | Process for producing vanillin |
| CN101417931A (en) * | 2008-11-28 | 2009-04-29 | 湖南阿斯达生化科技有限公司 | Synthetic method of ethyl vanillin and derivatives thereof |
| CN102010310A (en) * | 2010-10-21 | 2011-04-13 | 宁波王龙科技股份有限公司 | Productive technology of vanlillin by glyoxylic acid method |
| US20130123546A1 (en) * | 2010-06-11 | 2013-05-16 | Alma Mater Studiorum Universita Di Bologna | Production of aldehydes by oxidation in aqueous medium with selective recovery of the product by means of pervaporation |
| CN203750527U (en) * | 2014-03-14 | 2014-08-06 | 沅江华龙催化科技有限公司 | Multistage continuous reaction separation and synchronization device |
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| US3920750A (en) * | 1974-03-21 | 1975-11-18 | Int Paper Canada | Process for producing vanillin |
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| US20130123546A1 (en) * | 2010-06-11 | 2013-05-16 | Alma Mater Studiorum Universita Di Bologna | Production of aldehydes by oxidation in aqueous medium with selective recovery of the product by means of pervaporation |
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