CN87101031A - Be used to contain the extraction equipment and the method for solid particle or viscous feed liquid - Google Patents

Abstract

A kind of multi-stage continuous extraction device that has suspension, sediment or viscous feed liquid that is applicable to.This device is made up of the last settling section that joins together, following settling section and extraction section, and have a high dispersive device of material liquid entrance device and external enwergy input, apply oleophilic drainage section bar matter at each section of device inwall, the grid type filler of one group of surface for hydrophilic and lipophilic material arranged respectively in the upper and lower settling section, in following settling section bottom one solid outlet is set, forms the extraction equipment structure of three outlets of two imports.This device adopts the method for operating of paraphase extraction.The present invention can solve liquid-liquid extraction and liquid-solid extraction is carried out in same multitple extraction equipment.

Description

The present invention relates to the extraction equipment and the method for liquid solution, 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 solid contents such as lignin are 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.In the extraction as the guaiacol 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 folding except that all deciding ring and part rotating disks, 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 0.5, 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, also made extractant benzene become toluene solubility in raffinate to improve and increase and lost.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 heaviness again, 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 it is inapplicable that this technology need be carried out multitple extraction Shi And for sediment absorption solute, system for similar vanillic aldehyde is also inapplicable, and is more inapplicable when having the glue-like sediment.Because of can not solving, it in equipment, carries out continuous liquid liquid, liquid-solid multitple extraction, one 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 formed the high dispersive device that ， And has material liquid entrance device and external enwergy input by the last settling section that joins together, following settling section and extraction section.This container has vertical cylinder type limit wall, the inverted cone that its bottom tilts to the container vertical axis from the limit wall, and 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, and the material of inner wall surface coated oleophilic drainage influences operation to stop solid particle or glue-like resin to bond, gather in the equipment inner wall surface.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, carries heavy phase secretly in preventing gently mutually.Last settling section below is the inverted cone that tilts to the cylinder axis, links with the extraction section upper end.

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.

Settling section is and the identical cylindrical container of last settling section diameter under said, and inner wall surface also should be an oleophilic drainage section bar matter, and And one group of surface of part device within it is the grid type filler of lipophilic material, 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 a σ/aC＜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, and it is the mass-transfer efficiency height as a result, divides interval velocity fast.The present invention has simultaneously adopted the mechanical device of high dispersive ability, has improved dispersed phase drop or Dispersion of Solid Particles degree, makes drop be in frequent dispersion and state of aggregation, and 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, under the controlled situation of interface location, the discharging of solid phase can not influence normally carrying out of extracting operation like this.

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) be the upper settling section of cylindrical tube, 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) be the extraction section of columniform cylindrical shell, 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; (8) be with the angled level meters of horizontal level on lower interface, light phase entrance (17) device is between this two interface, (9) are level meters; (13) be 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 porch is 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, and PH1～2 have the glue-like resin, is solvent with benzene or toluene in the extraction, is 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, when blowing, should turn down the outlet valve aperture of raffinate liquid phase, for keeping 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, and the 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%.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

3%, solid phase does not have the bonding phenomenon in equipment, very good with separating of liquid phase yet.

Claims (8)

1, a kind of multi-stage continuous extraction device that is used for suspension, sediment or viscous feed liquid, it forms the high dispersive device that And has material liquid entrance device and external enwergy input by the last settling section that fuses, following settling section and extraction section, 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, at following settling section one solid Chen Jiang Qu And is set a solid outlet is set in the bottom, form the extraction equipment structure of three outlets of two imports.

2, extraction equipment as claimed in claim 1 is characterized in that heavy liquid inlet in extraction section manages on the light phase inlet tube in the upper and lower settling section pre-distribution hole is arranged.

3, 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 that can regulate temperature.

4, extraction equipment as claimed in claim 1 is characterized in that near the device interface meter 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.

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

6, the method for operating of extraction equipment as claimed in claim 1 is a kind of continuous paraphase extracting process, it is characterized in that elder generation by gently being full of container mutually, and charging when weight is identical then forms the paraphase extraction, and the interface of two-phase is at following settling section position.

7, continuous paraphase extracting process as claimed in claim 6 is characterized in that adopting high-frequency or high-revolving mechanical dispersion process.

8, continuous paraphase extracting process as claimed in claim 6 is characterized in that weight is in a ratio of 0.5～2.5.

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