CN1017214B - Extraction device and method for liquid with granules or high viscosity - Google Patents

Abstract

The present invention relates to a multistage continuous extraction device for suspended substances, precipitates or viscous material liquid. The device is composed of an upper settling section, a lower settling section and an extraction section which are connected, and is provided with a material liquid inlet and outlet device and a high dispersing device, wherein external energy can be input to the high dispersing device. Oleophilic and hydrophobic section bar is coated on the inner walls of the sections of the device, one set of grid type filling materials of which the surface has the oleophilic and hydrophobic section bar is respectively put in the upper settling section and the lower settling section, a solid outlet is arranged at the bottom of the low settling section, and thus, an extraction device structure with two inlets and three outlets is formed. The device adopts an operation method of phase reversal extraction. The present invention can simultaneously carry out liquid-liquid extraction and liquid-solid extraction in the same multistage extraction device.

Description

Extraction device and method for liquid with granules or high viscosity

The present invention relates to the extraction equipment and the method for solvent, liquid-liquid extraction and liquid-solid extraction are carried out in same multitple extraction equipment continuously, be applicable to and have the system that generates with solid phase in suspension, sediment or the extraction process, also can be used for the liquid-liquid extraction of viscous feed liquid, especially handle the feed liquid that has the glue-like resin and more can show its superiority.

Normally carry out the technical process more complicated respectively for the extracting process that has suspension, sediment or generate with liquid-liquid extraction and liquid-solid extraction with solid phase.Liquid-solid extraction can only intermittently operated, if it is agglomerating to meet the solid particle bonding, then liquid-solid extraction efficient is very low.Also handlebar liquid liquid and liquid-solid while extract in rotating disc column, as in acidic oxidation liquid, extracting vanillic aldehyde, adopt the positive extraction process, promptly be continuous phase with the water, organic facies is a decentralized photo, but when the lignin equal size is higher, the liquid liquid two phase stratification time is long, and operating difficulties must add surfactant, divide interval velocity though can improve like this, but increased the transmission resistance of solute, the mass transfer overall coefficient has been descended, if the contents of precipitate in the feed liquid further increases, also be difficult to layering even add surfactant, extracting operation just can't carry out.Create as Yu in the extraction of wooden phenol method synthesis of vanillin, owing to there is the glue-like solid sediment, not only adsorb vanillic aldehyde, make it be difficult to come together and, and in the equipment inner accumulated, choking phenomenon occurs, operation is promptly interrupted, extraction again after must cleaning.Be prolong operation cycle, have to remove and all decide the loop section rotating disk, so not only back-mixing is serious, and the ability drop of dispersant liquid drop, extraction efficiency is then very low, every meter theoretical stage of this tower only is 0.5, and ratio of solvent is but up to 4, and the vanillic aldehyde content (in total aldehyde amount) in the raffinate solid phase still is 10%～20%.Also must add another kind of etoh solvent simultaneously,, reduce sediment, be convenient to extraction to improve the solubility of resinoid in water.This had both consumed a large amount of ethanol, and extractant benzene or toluene solubility in raffinate is improved and the loss increase.In industrial production, the device of also useful differential extraction tower is realized this unit operations.But this equipment can only intermittently operated, and extract chronic, be more than four times of continuous extraction operation, equipment is stupid again gets, and floor space is big, particularly the solvent internal circulating load is big, ratio of solvent is more than 5.5, and corresponding solvent proportion of goods damageds resin total amount high and that enter in the extraction phase increases, and directly influences the recovery rate of vanillic aldehyde in follow-up vacuum distillation operation, compare with continuous extraction process, lose vanillic aldehyde about 5% more.

Chinese patent 85100841 has been introduced mixed clarifier after a kind of improve can carry out the liquid-liquid extraction that produces with solid phase, the problems referred to above have partly been solved, the liquid phase that produces in the solvent extraction process and the separation problem of relatively large solid phase precipitation thing have particularly been solved, make the precipitation discharge process not influence normally carrying out of extracting operation, but this technology is for need carry out multitple extraction because of sediment absorption solute the time and inapplicable, system for similar vanillic aldehyde is also inapplicable, more inapplicable when having the glue-like sediment, because of can not solving, it in same equipment, carries out continuous liquid liquid, liquid-solid multitple extraction, the sediment collector that volume is less with container shapes is similar is set below the container of this known extraction equipment in addition, make the precipitation that has heavy phase enter sediment collector, and make liquid-solid separation and precipitate coalescent, and then by solid phase outlet intermittent discharge sediment by valve control.But this sediment for glue-like just is difficult to operate, and because of the glue-like sediment can accumulate on the member in the device very soon, and passage, and makes the operation disruption can not ordinary production.

The objective of the invention is to overcome the shortcoming of above-mentioned known technology, a kind of extraction efficiency height is provided, can be suitable for the multi-stage continuous extraction apparatus and method that have suspension, sediment or viscous feed liquid again, can solve liquid-liquid extraction and liquid-solid extraction carries out in same multitple extraction equipment, solve the separation problem of raffinate liquid phase and raffinate solid phase simultaneously, especially for the system that has the glue-like solid, more can show its superiority, can or not gather owing to the bonding of solid particle influences normal running.

Device of the present invention is by the last settling section that joins together, following settling section and extraction section are formed, and have a high dispersive device of material liquid entrance device and external enwergy input, this container has vertical cylinder type limit wall, the inverted cone that its bottom tilts to the container vertical axis from the limit wall, solid phase outlet is set up on the summit of inverted cone, forms the extraction equipment structure of three outlets of two imports.

Said upward settling section is the cylindrical container of diameter greater than extraction section; the material of inner wall surface coated oleophilic drainage; to stop solid particle or glue-like resin to bond in the equipment inner wall surface; gather and influence operation, end device overfall on the outer wall, i.e. light phase export; one group of surface of last settling section interior arrangement is the grid type filler of hydrophilic material; carry heavy phase secretly in preventing gently mutually, last settling section below be the inverted cone that tilts to the cylinder axis, and links on the extraction section.

Said extraction section is the cylindrical container of diameter less than upper and lower settling section, inner wall surface is the material of oleophilic drainage, extraction section inside is provided with drop and disperses member, can adopt the various ways such as the well-known stirring of personnel, vibration, pulse of this technical field, but the annulus baffle plate that reduces back-mixing must be set, to prevent the decline of column efficiency, said whole component surface should be oleophilic drainage section bar matter.The heavy liquid inlet is set on extraction section Bian Bi top takes over, pre-distribution hole should be arranged on the heavy liquid inlet pipe in container, pre-dispersed in order to dispersed phase drop.

Said settling section down is and the identical cylindrical container of last settling section diameter that inner wall surface also should be an oleophilic drainage section bar matter, and one group of surface of part device is the grid type filler of lipophilic material within it, to prevent carrying light phase in the heavy phase secretly.Following settling section top is the circular cone that tilts to the cylinder axis, links with the extraction section lower end.Following settling section Bian Bi top is provided with light phase inlet connection, on the light phase inlet tube in container pre-distribution hole should be arranged, in order to the uniformity of continuous phase fluid on tower section.Near device interface meter gently entering the mouth mutually, level meters are taken over horizontal level is angled and are inclined upwardly, and take over passage to prevent that solid-phase material from blocking.Wall middle part, following settling section limit is provided with heavy out and takes over.Following settling section bottom is the inverted cone that tilts to the cylinder axis, and the bottom is the decanting zone, at its summit installing solid phase discharge connection.Solid decanting zone and the solid outlet of following settling section below partly are provided with heating jacket, and with hot water or water vapour heating, temperature can be regulated arbitrarily, so that the mobile performance when increasing solid phase and exporting.

The oleophilic drainage material of said each section inwall is non-metal linings such as polytetrafluoroethylene (PTFE), nylon, fiber glass epoxy, polypropylene etc., preferably polytetrafluoroethylene (PTFE).

For the decentralized photo solvent is a continuous phase, solute was the extraction process of three outlets of one two imports by the continuous paraphase extracting process that decentralized photo transmits to continuous phase with the water in employing when device of the present invention was operated.Elder generation is full of container by light phase (solvent), and light then, heavy phase charging simultaneously forms the paraphase extraction, and the interface of two-phase is at following settling section position.Heavy phase is dispersed in the continuous phase (light phase) with the drop state like this, and in order to the raising of mass-transfer efficiency, solid phase particles is enclosed in the drop, is difficult for the bonding tower member and influences operation.Light with the discharging of overflow mode, the flow by the discharging of valve regulated heavy phase is to control interface location.The solid phase discharging is controlled intermittent discharge by valve, suitably reduces the heavy out flow during discharging, and is constant to keep interface location.That adopts the inventive method gently, heavily is in a ratio of 0.5～1.5.Drop process for dispersing of the present invention adopts well-known high-frequency vibration in this technical field, pulse or high rotating speed stirring method.

The invention has the advantages that: one, the component surface that contacts with feed liquid at each section inwall of extraction equipment is after the specially treated of coated oleophilic drainage section bar matter, and the dispersion that had both helped the drop phase has improved mass-transfer efficiency; Make hydrophilic solid particle of aqueous phase or glue-like resin be difficult to gather, thereby operation can be carried out smoothly again in element of installation surface bonding.

Two, adopt paraphase extracting process solid particle to be enclosed among the dispersed phase drop, be accumulated into bulky grain with regard to difficult collision between the solid granule, being easy to come together by the adsorbed solute of solid particle like this, and the solid particle that is enclosed in the drop is difficult to contact the back deposition and blocking channel with element of installation.

Three, for common α δ/α C＜0 system, when mass transfer direction during from decentralized photo to continuous phase, the self-cohesion action between the drop is strengthened, and helps the raising of mass transfer rate, and divides interval velocity fast, is difficult for carrying secretly, is convenient to operation.When transmitting toward the low viscosity direction from high viscosity for high solid content, full-bodied feed liquid, solute, liquid film plays pendulum, it is the mass-transfer efficiency height as a result, divide interval velocity fast, the present invention has simultaneously adopted the mechanical device of high dispersive ability, improved dispersed phase drop or Dispersion of Solid Particles degree, made drop be in frequent dispersion and state of aggregation, extraction efficiency significantly improves.

Four, set up solid decanting zone and solid outlet, form the extraction equipment structure of unique three outlets of two imports, this is handled easily both, is difficult for blocking the outlet conduit of raffinate water again.Solid phase in the decanting zone of setting up with the water layering, the continuous blow-down of raffinate water, the solid phase intermittent discharge, like this under the controlled situation of interface location, the solid phase discharging can not influence normally carrying out of extracting operation.

Five, with the mass-transfer efficiency height of method and apparatus of the present invention, the corresponding solvent load that reduced, so not only solvent consumption descends, and enters the total impurities minimizing of solvent, has brought convenience to post processing, has also improved the recovery rate in the subsequent technique process.

Accompanying drawing 1 is a structural representation of the present invention.

2 is the upper settling section of cylindrical tube, and its underpart is shaped as turbination, and the Bian Bichu of its top is provided with light phase overfall 1, the grid type filler 3 of one group of hydrophilic material of its interior arrangement; 6 is the extraction section of columniform cylindrical shell, and its wall place, limit, top is provided with heavy liquid inlet 4, and the place is provided with pre-distribution hole 5 in the heavy liquid inlet, the decentralized institution 7 of its interior arrangement heavy phase drop, and its surface should be oleophilic drainage section bar matter; The 8th, with lower interface on the angled level meters of horizontal level, light phase entrance 17 installs between this two interface, and the 9th, level meters; 13 is the lower settling section of cylindrical tube, its top is conical, its underpart is turbination, its wall place, limit, top is provided with light phase entrance 17, and light phase entrance 17 places are provided with pre-distribution hole 10, the grid type filler 11 of one group of lipophilic material of its interior arrangement, its wall place, limit, middle part is provided with heavy out 12, the heavy out bottom is decanting zone 16, in its bottom solid phase outlet 15 is set, and thereunder installs heating jacket 14. Extraction section 6, lower settling section 13 join together, each section inner wall surface coated oleophilic drainage section bar matter. Upper settling section 2, extraction section 6, lower settling section 13 joins together, each section inner wall surface coated oleophilic drainage section bar matter.

Be to use embodiments of the invention below:

Raw material is the condensation reaction solution of synthetic legal system vanillic aldehyde, and vanillic aldehyde (total aldehyde meter) concentration is about 128g/l, contains the acid solution of HCl.PH1～2 have the glue-like resin, are solvent with benzene or toluene in the extraction, are in a ratio of 0.5～1.5.The mechanical device of high dispersive ability is a reciprocating oscillating screen plate, sieve plate is made by polytetrafluoroethylene (PTFE), the component surface that contacts with material in the equipment is polytetrafluoroethylene (PTFE), the grid type filler of hydrophilic material titanium is set, the polytetrafluoroethylene (PTFE) grid type filler of device lipophilic in the following settling section in the last settling section.The extraction section operating temperature is 40～70 ℃, and following settling section heating jacket temperature is 60～100 ℃, and the amplitude of decentralized institution is 5～20mm, vibration frequency 150～400 times/minute.

During operation, be full of solvent in the tower earlier through preheating, open vibrating mechanism then, be adjusted to predetermined amplitude and frequency, add vanillic aldehyde condensation liquid and solvent more simultaneously through preheating, the outlet valve aperture of control raffinate liquid phase is to stablize the liquid-liquid two-phase interface position, carry the size of the measuring pump demonstration two phase flow of liquid, 70% when its numerical value is liquid flooding, raffinate solid phase baiting valve is interrupted to be opened, turning down the outlet valve aperture of raffinate liquid phase when blowing is corresponding, is to keep the liquid-liquid two-phase interface invariant position.

Extraction in this device, do not find solid-phase resin bonding and choking phenomenon through long period of operation, liquid liquid two phase stratification is fast, and be difficult for carrying secretly, extraction efficiency is up to 96%, improve more than 5% than common extracting process, vanillic aldehyde concentration improves in the extraction phase, greater than 120g/l, the solvent unit consumption descends 20%, and vanillic aldehyde content can be reduced to 0.5g/l in the raffinate phase, vanillic aldehyde content in the solid phase reduces more than 50% simultaneously, and the total amount that the impurity resin enters the solvent phase reduces about 60%, makes the recovery rate of post processing vacuum distillation improve 3%, and the extraction theory progression of this equipment is about 3 grades/meter.

Acidifying solution with PH4 lignin legal system vanillic aldehyde is a feed liquid, contains vanillic aldehyde 50g/l, and when other condition was pressed above-mentioned requirements, extraction yield was 23%, and solid phase does not have the bonding phenomenon in equipment, very good with separating of liquid phase yet.

Claims (4)

1, a kind of multi-stage continuous extraction device that is used for suspension, sediment or viscous feed liquid, it is made up of the last settling section 2 that fuses, following settling section 13 and extraction section 6, and have a high dispersive device 7 of material liquid entrance device and external enwergy input, it is characterized in that in each section inwall coated oleophilic drainage section bar matter, the grid type filler that the hydrophilic of one group of surface and lipophilic material are arranged respectively in last settling section and the following settling section, one solid decanting zone 16 is set and one solid outlet 15 is set at following settling section, form the extraction equipment structure of three outlets of two imports in the bottom.

2, extraction equipment as claimed in claim 1 is characterized in that solid decanting zone and the solid outlet below following settling section partly is provided with the heating jacket 14 that can regulate temperature.

3, extraction equipment as claimed in claim 1 is characterized in that near the device interface meter 9 light inlet mutually on the following Bian Bi top of settling section, and level meters are taken over horizontal line is angled and are inclined upwardly.

4, extraction equipment as claimed in claim 1 is characterized in that preferably polytetrafluoroethylene (PTFE) of each section inwall coated oleophilic drainage section bar material.

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