CN1226181A - Column and process for deodorising dispersions - Google Patents
Column and process for deodorising dispersions Download PDFInfo
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- CN1226181A CN1226181A CN97196719A CN97196719A CN1226181A CN 1226181 A CN1226181 A CN 1226181A CN 97196719 A CN97196719 A CN 97196719A CN 97196719 A CN97196719 A CN 97196719A CN 1226181 A CN1226181 A CN 1226181A
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- tower
- dispersion
- steam
- plate
- polymeric dispersions
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/16—Fractionating columns in which vapour bubbles through liquid
- B01D3/22—Fractionating columns in which vapour bubbles through liquid with horizontal sieve plates or grids; Construction of sieve plates or grids
- B01D3/225—Dual-flow sieve trays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/16—Fractionating columns in which vapour bubbles through liquid
- B01D3/22—Fractionating columns in which vapour bubbles through liquid with horizontal sieve plates or grids; Construction of sieve plates or grids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0005—Degasification of liquids with one or more auxiliary substances
- B01D19/001—Degasification of liquids with one or more auxiliary substances by bubbling steam through the liquid
- B01D19/0015—Degasification of liquids with one or more auxiliary substances by bubbling steam through the liquid in contact columns containing plates, grids or other filling elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/001—Removal of residual monomers by physical means
- C08F6/003—Removal of residual monomers by physical means from polymer solutions, suspensions, dispersions or emulsions without recovery of the polymer therefrom
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Treating Waste Gases (AREA)
- Housing For Livestock And Birds (AREA)
- Gas Separation By Absorption (AREA)
Abstract
In the counterflown column for lowering the residual volatile substance content of dispersions, having 5 to 50 vertical and/or transverse flow filter bases, the specific free aperture area in the vertical flow filter bases is 2 to 25 % and in the transverse flow filter bases 1 to 10 %, and the mean aperture diameter is 10 to 50 mm in the vertical and 2 to 10 mm in the transverse flow filter bases.
Description
The present invention relates to be used for reducing tower and method, the equipment of preparation polymeric dispersions, the polymeric dispersions that is obtained and the application thereof of the remaining volatile matter content of dispersion (dispersion deodorizing).
It is known adopting the method for suspension or emulsion polymerizing preparation compound suspension or dispersion.Usually, still comprise undesirable volatile organic component in the product, as the low molecular weight product that generates because of the catabolite that transforms the impurity that contains in incomplete and residual monomer, the raw material, initator or side reaction.These are referred to as remaining volatile matter below compound.December 15 nineteen ninety-five is by promulgation EC (European Community) environment code name is done among the decision 96/13/EC of the committee above-mentioned remaining volatile matter to be subdivided into VOC (VOC) and volatility aromatic hydrocarbons again with regard to interior paint and indoor coating regulation environmental standard.The both of these case indication all be that boiling point under condition of normal pressure (or initial boiling point) is up to 250 ℃ organic compound.Volatility aromatic hydrocarbons comprises at least one virtue nuclear in structural formula.The employed collective noun of this paper (term) " remaining volatile matter " is meant that all boiling points (or initial boiling point) are up to these organic compounds of 250 ℃.These remaining volatile matters are unwelcome to the occasion of many use dispersions and suspension, for example are used for food or cosmetic field or interior decoration, so, require as far as possible they to be removed.
So, the processing that need remove VOC to dispersion or emulsion.This class is handled and is referred to as deodorizing usually.Known have various technology and equipments to can be used for this purpose: except chemical method, but this class chemical method only works to unsaturated compound, and that generally adopts will calculate steam stripping technique, even a kind of stripping gas passes suspension or dispersion.Employed stripping gas comprises air, nitrogen, supercritical carbon dioxide, ozone or steam.With stripping gas suspension-treating or the used desirable various forms of equipment of dispersion.The simplest equipment of style is made of the container that fills suspension or dispersion, from the bottom of container entire container is introduced and passed to stripping gas by spray gun or valve.Alternatively, deodorizing of today also can be carried out in deodorizing tower or devolatilization tower continuously.
DE-A2550023 discloses a kind of devolatilization tower, and it comprises many column plates of laying from bottom to top.The key character of this tower is, vacates the gap equably between week of every block of column plate and shell.Yet this feature has but seriously hindered the efficient of whole tower, can just flow through from these edge voids under the situation that does not meet the requirements of Srteam Stripping effect because can observe liquid phase.
DE-C2759097 has described a kind of monomer methods of removing from dispersion, wherein employed tower almost completely has been full of liquid., can cause holdup capacity undesirably to increase like this, and the periodic cleaning that requires also takes a lot of work very much, cause when for example changing product and always go wrong.The ratio perforated area of this tower is 1.6%.
DE-C2855146 discloses a kind of removing monomer methods, and wherein sieve-plate tower operates in the state that is counter current contacting with steam, and the irrigation canals and ditches first class that makes aqueous dispersion flow through forming by side plate footpath.Opening diameter is 0.5～2 millimeter, is 0.04～0.0004% than perforated area.This kind column structure is still complicated, and holdup capacity is excessive, and cleaning is also taken a lot of work.
DE-C2521780 discloses a kind of by the tower removing monomer methods that sieve plate is housed, and this method adopts 100～150 ℃, 0.8～1.6 steam that clings to.The described method of this article exists the higher shortcoming that may damage product of Yin Wendu.This problem can soundd out by shortening the holdup time and offset.The steam injection rate is a benchmark with the dispersion scale of construction that adds, and is 1～5% (weight).DE-A2733679 has described a kind of similarity method that utilizes perforated plate tower to remove monomer, 90～150 ℃ of operations.In order to arrive said temperature, must improve the pressure in the tower usually.Except common existence such as cost of energy is higher the shortcoming, this method also exist since in the tower higher the causing of temperature can't process the temperature shortcoming of sensitive product comparatively.And, in disclosed method, can't use softening point to be lower than 90 ℃ polymer.Also mention in the literary composition, the distance between plates of this tower is smaller, because otherwise will occur polymer to a certain extent and hang over danger on the tower wall.Opening diameter is 10 millimeters, is 5.5～7.5% than perforated area.
Therefore, the objective of the invention is to find out a kind of improved method, it can overcome above-mentioned shortcoming and be adopted on technical simple, the cost economic method that remaining volatile matter is removed from aqueous suspension or dispersion.Meanwhile, it also should allow to adopt aborning higher steam flow rate, allow to handle the product comparatively responsive to temperature, and also can reach high-purity simultaneously, do not need significantly to increase the holdup time in the tower.Have again, a kind of countercurrent tower that provides, its is produced under allowing not establish the condition of recipient in addition in the upstream of tower, and the cleaning of tower also obtains simplifying, so replacement of products also just can be finished easily.
We find that this purpose can a kind ofly reduce that the countercurrent tower of remaining volatile matter reaches in the dispersion by being provided with, this tower comprises 5～50 double pass trays and/or single overflow sieve plate, wherein the ratio perforated area of double pass tray is 2～25%, the ratio perforated area of single overflow sieve plate is 1～10%, the average opening diameter of double pass tray is 10～50 millimeters, and the average opening diameter of single overflow sieve plate is 2～10 millimeters.
Purpose of the present invention is again to reach by a kind of method for preparing low remaining volatile matter content dispersion with the steam treatment dispersion in the countercurrent tower that comprises double pass tray and/or single overflow sieve plate, wherein steam and dispersion are counter current contacting, and the tower internal pressure is 0.1～0.7 crust therebetween.
In this equipment, the dispersion feed (amount) by perforated area is preferably 4～15 kilograms/square centimeter hours to double pass tray, and the single overflow sieve plate is preferably 15～25 kilograms/square centimeter hours.
Collective noun used herein " remaining volatile matter " has this paper to start the meaning of defined, and remaining volatile matter content is according to DRAFT international standard (draft) IOS/DIS13741, and first adopts gas chromatography to measure.In this standard, remaining volatile matter is meant residual monomer and other organic compounds.Concrete example is an acrylate, as n-butyl acrylate and isobutyl acrylate; Methacrylate is as methyl methacrylate; Acrylonitrile; Butadiene; Styrene; Vinyl acetate; Vinyl chloride; Also has accessory substance, as acetaldehyde and ethylbenzene.Propionitrile, ethyl acrylate and 4 vinyl cyclohexene have also been enumerated.
According to method of the present invention, can adopt better simply structural design and method cost economy simple from aqueous suspension or dispersion, to isolate monomer with technology.Since simplicity of design, thereby holdup capacity is lower, and this tower proves that in practical operation running is reliable, is easy to cleaning, even it is also comparatively simple to change product.In addition, higher plate efficiency can be reached, thereby the quantity of column plate can be reduced.Because the tower internal pressure reduces, and then temperature is also just lower in the tower, even therefore temperature sensitive dispersion also can be handled.This method also allows to take higher steam flow rate, and the ruckbildung of polymer can be relieved to the degree that does not hinder separation process to carry out in suspension or the dispersion.
Below, at first illustrate according to countercurrent tower of the present invention and comprise the device of this tower, the corresponding new method of subsequent discussion and thus obtained according to dispersion of the present invention and even its application.
Countercurrent tower
Significantly different with known countercurrent tower, novel countercurrent tower of the present invention is operable under the very high output, and therefore, tower itself can be made very for a short time.This just helps the cleaning of tower.
In view of present countercurrent tower is just obtaining increasingly extensive application, be not limited only to be the deodorizing of particular type dispersion, and a part that is taken as the fecund product device that relates to frequent replacing product or dispersion operates, and wishes that therefore employed tower clears up simply.Whether tower is cleared up to such an extent that thoroughly the quality to obtaining dispersion is most important.Scale removal process is simplified and accelerated to tower by the present invention's design, and the cleaning Fluid Volume that needs is also less.This just makes the running cost of this tower reduce greatly, thereby is applicable in the frequent fecund product device of changing product and uses.Because cleanup step is simple especially, preferred employing comprises the tower of double pass tray in fecund product device, rather than also spendable single overflow sieve-plate tower.
Can comprise the combination of double pass tray, single overflow sieve plate or double pass tray and single overflow sieve plate according to tower of the present invention.Preferably, tower of the present invention or comprise double pass tray perhaps comprises the single overflow sieve plate.In this connection, plate number is 5～50, is preferably 8～40, preferred especially 15～30.In this respect, tray spacing is preferably 250～800, and is preferred especially 300～700, especially preferred 400～600 millimeters.Tower height is preferably 6～25, preferred especially 10～20 meters.Tower section is preferably circle, and its diameter is preferably 400～2500 millimeters, preferred especially 800～1600 millimeters.The average opening diameter of double pass tray is 10～50, is preferably 12～25 millimeters.Under the situation of single overflow sieve plate, average opening diameter is 2～10, and preferred 4～8 millimeters, the hole of being opened is preferably circular.Than perforated area, i.e. perforate accounts for the percentage of every column plate area, and being suitable under the situation of double pass tray is 2～25%, is preferably 5～20%, and preferred especially 10～18%; Being suitable under the situation of single overflow sieve plate is 1～10%, is preferably 3～8%, preferred especially 4～7%.
In this respect, be one to guarantee the dispersion feed flow rate that below the steam flow rate condition of regulation is issued to, will mention than the preferred standard of perforated area by perforated area.
No matter the cross sectional shape of tower still is that the shape of perforate can be adjusted according to concrete requirement.They are preferably circular tower section or round hole, although for special occasions, other shapes may be suitable.
The general considerations of single overflow sieve plate and double pass tray and design thereof can be seen in KlausSattler, and " thermal Release Technology ", VCH, 1988 (the 172nd page, Fig. 2～59; The 174th page, table 2～19).
Preferably, the tower diameter of this novel tower is what enlarge on top, so that realize the purpose that the dispersion drop separates with steam by gravity.The diameter of this expanding reach is 1 meter at least, particularly under the situation of trourelle.Maximum can reach 4 meters, especially under the situation of big tower.Usually, the top amplification quantity is about 1.5 times of column plate diameter.
Preferably, this tower has 1～3 meter in its bottom zone in addition, and preferred 2～3 meters extension is promptly as at the bottom of the tower.At the bottom of this tower in order to accept the dispersion after the deodorizing.This part dispersion is as the pump charging of being sent to subsequent handling.
Dispersion adds from (top) portion of the going up district of tower, preferably from upper zone (top expanded section) adding of the expansion of tower.
According to the present invention, the preferred tower that comprises double pass tray that uses, because it does not have any dead zone relevant with style, in other words, cleaning is got up laborsaving, the efficient height.As a result, the size of tower, particularly tower height and plate number all can reduce.It is 15～30 blocks of column plates of 400～600 millimeters that this tower preferably includes spacing, and tower diameter is 800～1600 millimeters, especially 1000～1500 millimeters.The ratio perforated area of tower and the selection principle of diameter are to make the throughput of dispersion, specifically between 5～30 tons/hour, by the dispersion feed flow rate of the perforated area scope between 4～15 kilograms/square centimeter hours.
The single overflow sieve-plate tower preferably has external dimensions and the number of plates identical with double-current tower.The ratio perforated area of tower and the selection principle of diameter are to make the throughput of dispersion, specifically between 10～30 tons/hour, by the dispersion feed flow rate of the perforated area scope at 15～25 Kilograms Per Square Meters hour.
Preferably has (overflow) weir according to tower of the present invention.Height of weir is preferably 50～200 millimeters.The downcomer outlet port height of tower is preferably 20～50 millimeters, preferred especially 25～40 millimeters.Than perforated area is about 6%.The number of aperture of every block of plate is 2000～9000.
Can constitute one with the equipment of preparation polymeric dispersions according to tower of the present invention.The post-reactor (B) that this kind new type of polymer dispersion preparation facilities comprises reactor (A), may also have, as above-mentioned tower (C), exhaust steam heat exchanger (D) and possible decompressor (E), filter (F) and adjusting device (G).In this kind arrangement, the outlet of reactor (A) or post-reactor (B) is preferably direct, and promptly the centre is not established receiver in addition, is connected to the import of tower (C).This kind device is shown in the drawings, wherein
Fig. 1 schematically represents to comprise the device of double-current tower, and
Fig. 2 schematically represents to comprise the device of single overflow sieve-plate tower.
Employed code name meaning is as follows among the figure:
A: the polymer reactor of belt stirrer
B: post-reactor
C: countercurrent tower has
C1: cat head expanding reach
C2: double pass tray (Fig. 1) and single overflow sieve plate (Fig. 2)
C3: at the bottom of the tower
D: exhaust steam heat exchanger
E: pressure-reducing station has
E1: steam (vapor) outlet reaches
E2: dispersion outlet
F: filter
G: device
Usually, dispersion is by batch technology preparation discontinuously in reactor (A), and material wherein is transferred in the post-reactor through after being generally incomplete conversion.According to method in the past, dispersion must be transferred to independent receiver from post-reactor (B), and then joins in the deodorizing tower.Why must do like this, be because the thruput of the tower thruput that (B) discharges much smaller than pump from post-reactor is.Novel tower (C) then preferably allows sufficiently high thruput to pass through, so that can allow dispersion directly send in the tower (C) during post-reactor (B) emptying, because this tower can be handled and post-reactor (B) identical thruput in evacuation procedure.And owing to can not establish receiver in addition, so whole device just obtains simplification, and then better cost benefit is made.And since no longer include the individual receivers that needs control, whole operation also obtains simplifying.Those parts that or not influenced by tower in device, target are the flow pumpings with 20～50 tons/hour.At this moment, can save the receiver of tower upstream or intermediate buffering jar under for about 10 tons/hour condition directly from post-reactor charging to this tower in the thruput of tower.
Usually, pressure-reducing station (E) is set, so that can adjust to the dispersion water content of at the bottom of tower, discharging.Condensation can take place in part steam usually that be introduced in tower, thereby the water content of dispersion is higher at the bottom of the tower.In order to reduce this water content, can make the dispersion of acquisition further reduce pressure (reducing pressure) by vacuum equipment, part water is discharged with the form of steam (E1) in decompression process.So, the dispersion (E2) of discharging from pressure-reducing station (E) just is adjustable to the water content of requirement.
This method
Above-mentioned tower and device are applied in the new method of the present invention by favourable mode, to prepare the dispersion of low remaining volatile matter content.In this new method, the dispersion that obtains from reaction is generally polymeric dispersions, be preferably aqueous polymer dispersion, by tower, steam passes through under the tower press strip spare of 0.1～0.7 crust according to the direction that is adverse current with dispersion in the mode that is counter current contacting with steam.When using polymeric dispersions, the preferred settings value of tower internal pressure should guarantee that tower top temperature is higher than the glass transition temperature of polymer, the while column bottom temperature is lower than polymeric dispersions and will loses its stability, thereby the temperature such as decomposition or agglomeration or flocculation takes place.
The tower internal pressure is preferably at 0.2～0.7 crust, and special preferably is 0.2～0.5 crust in addition at the cat head place.
Temperature is preferably 50～90 ℃ in the tower, and particularly preferably in 60～82 ℃, wherein tower top temperature is lower than at the bottom of the tower, and this is because the cause that exists pressure to fall in the tower.The inlet temperature of dispersion is preferably 50～90 ℃, preferred especially 60～80 ℃.Column bottom temperature is preferably 70～90 ℃.The dispersion outlet temperature is suitable with this temperature.Tower top pressure is 0.2～0.5 crust, is 0.3～0.7 crust more than at the bottom of the tower.
The design data of double flow tray tower for example is: 15～25 millimeters of opening diameters, area load 8～15 cubic metres/square metre hours, by the ratio load in perforate cross section 10～12 kilograms/square centimeter hours, tower top pressure 0.2～0.5 crust (absolute pressure).
The design data of single overflow sieve-plate tower for example is: about 4 millimeters of opening diameter, area load 8～15 cubic metres/square metre hours, than perforated area 5～10%, 100～200 millimeters of heights of weir, tower top pressure 0.2～0.5 crust (absolute pressure), by the ratio load in perforate cross section 15～22 kilograms/square centimeter hours.
Steam utilization factor according to the inventive method is measured according to the water yield that with the dispersion weight of introducing is benchmark, is preferably 10～50%, preferred especially 20～30% (weight).
The steam throughput is preferably about 0.1～10 ton/hour, preferred especially 1～8 ton/hour.The dispersion throughput is preferably 1～50 ton/hour, preferred especially 5～30 tons/hour.The dispersion throughput is preferably 20 tons/hour or higher in the tower that production scale is used, and is 5～10 tons/hour in small-scale production, and in pilot-plant scale (experimental stage), is about 1～2 ton/hour.This throughput depends on the diameter of tower.
The specific area load of tower is 1.6～25, preferred 8～15 cubic metres of dispersions/square metre tower section area/hour.
Feed flow rates by perforated area is preferably 4～15 to double pass tray, preferred especially 10～13 kilograms/square centimeter hours, the single overflow sieve-plate tower is preferably 15～25, preferred especially 15～22 kilograms/square centimeter hours.
Operator scheme according to the inventive method allows to adopt high ratio throughput in tower.Therefore, the size of tower can maintain very little level, and this at first makes equipment can design to such an extent that more meet the cost benefit principle, secondly can reduce the interior surface area of tower, and the latter can reduce the needed cleaning work amount of product of changing again.
Under the condition of given stripped vapor to the dispersion weight ratio, than liquid load (dispersion load) height, gas load is just high, and then the flow velocity in the gas-phase space is also just high.Thereby can suppress to form on the plate stable foam, preferably can avoid substantially.Foam usually causes tower, downstream separator and vacuum equipment duty not normal, thereby does not wish to occur.This novel tower and new method, owing to can suppress to foam, thereby additional foam separator or bulb-breaking device might be saved.
Adopt the new method of this novel tower can be with the summation of remaining volatile matter content, with the total dispersion weight is benchmark, be reduced to the following numerical value of 100ppm, usually even be low to moderate below the 50ppm, under favourable situation even be lower than 25ppm, the degree of this reduction simultaneously also can be adjusted to the specific numerical value that requires by the structural design and the technology controlling and process of tower.In preferred tower operator scheme continuously, the holdup time in the tower, according to the difference of employed dispersion, preferably between 100～2000 seconds, special preferred 200～1000 seconds in addition, especially preferred 400～800 seconds.Regulate throughput, steam load and vapor (steam) temperature or pressure, and regulate set plate number, the dispersion purity that just can obtain requiring.Particularly preferred single overflow sieve-plate tower combination of process parameters is such:
-to the situation of 1～1.5 meter of tower diameter, the dispersion throughput is 10～25 tons/hour,
2.5～7.5 tons/hour of-steam throughputs,
Gas flow rate 40～140 meter per seconds in the-hole,
Gas velocity 2.5～10 meter per seconds in the-pipe.
This new method can be utilized the high advantage of plate efficiency.When using double pass tray, accessible plate efficiency is with relevant based on the throughput in perforate cross section, this plate efficiency preferably 7.0～above 30% scope.Under the situation of single overflow sieve plate, plate efficiency preferably is up to 20%.Determine that the method for plate efficiency will explain in the example hereinafter.
The invention still further relates to can be according to the dispersion of this new method preparation.This is that remaining volatile matter content is lower than 100ppm, usually even be lower than 50ppm, under favourable situation even be lower than the dispersion of 25ppm, refers in particular to polymeric dispersions, can be according to above method preparation.The regulation that the composition of preferred dispersions is seen below.
Dispersion
The dispersion of using in this new method can be any dispersion that can remove the remaining volatile matter of contents level that comprises.The example of this kind dispersion for example is dispersion, the inorganic particle dispersion of contaminated soil, the dispersion of biomolecule dispersion, particularly organic compound, especially polymer, and these dispersions are aqueous dispersion preferably.
The aqueous polymer dispersion that is particularly useful for the inventive method is such fluid system, and it comprises the polymer beads that stable dispersion distributes that is as decentralized photo in the aqueous dispersion media.The diameter of this polymer beads is general main to be distributed in 0.01～5 micron, often mainly at 0.01～1 micron.The stability of this dispersion distribution often can be kept at least one month, in many cases even reach at least 6 months.
The situation of polymer solution is such when evaporating just as solvent, aqueous polymer dispersion also has the tendency that forms polymer film when aqueous dispersion media is evaporated, this reason that also why aqueous polymer dispersion can be coated with as adhesive in every way just, as be used to be coated with the coating or the compound of leather.
In principle, with regard to aqueous polymer dispersion, should distinguish a moisture secondary dispersion and a moisture dispersion.Moisture secondary dispersion is that those polymer in its preparation process are to generate beyond aqueous dispersion media, for example in the solution of the nonaqueous solvents that is suitable for.This solution is transferred in the aqueous dispersion media subsequently, then, and along with the carrying out of dispersion process driven away this solvent, usually by distillation.Obviously different therewith, a moisture dispersion is that those polymer directly generate the dispersion of disperseing distribution form in the middle of aqueous dispersion media itself.The basic common ground that ownership Preparation Method is had is that the formation of polymer all relates to uses the monomer with at least one ethylene linkage unsaturated group uniquely, perhaps uses with other materials.
The monomer that this kind has at least one ethylenically unsaturated group is combined into that the process of polymer normally finishes by initiated polymerization, and the character of initiation especially depends on makes it to satisfy these features to the desired performance characteristic of purpose product.The example that can enumerate comprises that ion and free radical cause.Yet this combination also can cause similar polymerisation by catalyst action and finish.What especially often use is that free radical causes, and when carrying out the free radical initiation, the monomer that contains ethylenically unsaturated group is in conjunction with normally: under the situation of a moisture dispersion, adopt free radical aqueous emulsion polymerisation to realize, and under the situation of moisture secondary dispersion, then adopt the free radical solution polymerization reaction to finish.
Can select polymerizing condition to meet the requirements of polymer features, as molecular weight, molecular weight distribution and the degree of branching.If purpose is to make to be swift in response and finishes, but this generally is worthless, just allows reaction proceed to until finishing.So the aqueous polymer dispersion that is obtained after the reaction still contains monomer, particularly ethylenically unsaturated monomer.Because ethylenical unsaturated double bonds is active higher in this type of residual monomer such as acrylonitrile and vinyl acetate, they are not overall safeties on toxicology, therefore should remove from dispersion.This purpose can adopt the present invention to reach.This method is applicable to any polymer that is dispersed in the water-bearing media, no matter which kind of type this polymer belongs to.In view of the above, term " polymer " used in the present invention " both contained condensation polymer, as polyester, addition polymers such as polyurethane, also contain the polymer that can obtain via ion or radical polymerization.Adopt the hybrid mode of above-mentioned synthetic method can produce suitable dispersion used according to the present invention equally, copolymer also is the same.
The preparation method of the aqueous polymer dispersion of various above-mentioned polymer types is known, as rolling up referring to " polymer science and engineering complete works " the 8th, from the 659th page (1987); D.C.Blackley, " high polymer latex ", the first volume is from the 35th page (1966); H.Warson " synthetic resin emulsion application ", the 246th page is played the 5th chapter (1972); [publisher is not quite clear] D.Diederich, " modern chemistry " 24 phases, the 135th～142 page (1990); " emulsion polymerisation ", international scientific publishing company, New York (1965); DE-A4003422 and " dispersion synthetic high polymer ", F.Holscher, Springer publishing house, Berlin (1969).
Be applicable to the monomer that at least one monoene belongs to unsaturated group that has of this new method, comprise that especially the monomer of radical polymerization can directly take place for itself, for example: alkene such as ethene; Vi-ny l aromatic monomers is as styrene, AMS, chloro styrene or vinyltoluene; Vinyl alcohol and the monocarboxylic ester that contains 1～18 carbon atom are as vinyl acetate, propionate, vinyl propionate, vinyl laurate, new vinyl acetate acid and stearic acid vinyl ester; And as monomer VEOVA9～11 (VEOVA means the trade name of Shell Co. Ltd, means vinyl carboxylates, also is called Versatic X acid) of supply of commodities; α, β-monoene belongs to unsaturated monobasic and dicarboxylic acids, preferably have 3～6 carbon atoms, as acrylic acid, methacrylic acid, maleic acid, fumaric acid and itaconic acid, with have 1～12 usually, preferred 1～8, the especially ester of the alkanol of 1～4 carbon atom, for example methyl esters of acrylic acid and methacrylic acid, ethyl ester, positive butyl ester, isobutyl ester, the tert-butyl ester and 2-Octyl Nitrite, dimethyl maleate or n-butyl maleate; α, the nitrile of β-monoethylenically unsaturated carboxylic acid such as acrylonitrile; And C
4-8-conjugated diene such as 1,3-butadiene and isoprene.Under unique situation that is prepared aqueous polymer dispersion by the free radical aqueous emulsion polymerisation process, these monomers form first kind of monomer usually by accounting for more than 50% (weight) by the monomer total amount that the free radical aqueous emulsion polymerisation process is carried out polymerization.Usually, these monomers are only medium to being slightly soluble in water under standard state (25 ℃, 1 atmospheric pressure).
Under above-mentioned state, the example of the higher monomer of solubility comprises α in the water, β-monoene belongs to unsaturated monobasic and dicarboxylic acids and acid amides thereof, as acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, acrylamide and Methacrylamide, also have vinyl sulfonic acid and water soluble salt and N-vinyl pyrrolidone.
Prepare under the situation of aqueous polymer dispersion by the polymerization of free radical aqueous emulsion unique, have higher water miscible above-mentioned monomer and only participate in copolymerization usually as modified monomer, its consumption, by the monomer total amount for the treatment of polymerization, less than about 50% (weight), be generally 0.5～20, preferred 1～10% (weight).
Usually the monomer of intensity in the aqueous polymer dispersion film forming be can increase, at least one epoxy radicals, hydroxyl, N-methylol, carbonyl or at least two non-conjugated ethylenical unsaturated double bonds usually comprised.The suitable example of this class is: the α that comprises 3～10 carbon atoms, the N-alkanamides of β-monoethylenically unsaturated carboxylic acid, and these acid and the ester that comprises the enol of 1～4 carbon atom, in the middle of this, N hydroxymethyl acrylamide and N-methylol methacrylamide are particularly preferred; Comprise the monomer of two vinyl, the monomer that comprises the monomer of two ethenylidenes and comprise two alkenyls.
Special in this respect advantageously dihydroxy alcohol and α in addition, the diester of β-monoethylenically unsaturated monocarboxylic, wherein acrylic acid and metering system acid diesters are preferred.The example that comprises this type of monomer of two non-conjugated ethylenical unsaturated double bonds is: the diacrylate of aklylene glycol and dimethylacrylate, as glycol diacrylate, 1,3-butanediol diacrylate, 1,4-butanediol diacrylate and propylene glycol diacrylate, divinylbenzene, metering system vinyl acetate, vinyl acrylate, ALMA, acrylic acid allyl ester, maleic acid diallyl ester, fumaric acid diallyl ester, methylene-bisacrylamide, acrylic acid cyclopentadiene ester or cyanuric acid triallyl ester.Particular importance also has in this respect: methacrylic acid and acrylic acid C
1～C
8Hydroxy alkyl ester, as acrylic acid and the positive hydroxyethyl ester of methacrylic acid, positive hydroxypropyl ester or positive hydroxyl butyl ester, and such as DAAM and acrylic acid acetoacetyl ethyl ester methacrylic acid acetoacetyl ethyl ester, methacrylic acid urea ethyl ester and acrylamido glycolic compounds.Prepared under the situation of aqueous polymer dispersion by the free radical aqueous emulsion polymerisation process uniquely, the consumption of above-mentioned monomer in copolymerization by treating the polymerization single polymerization monomer total amount, is 0.5～10% (weight).
In free radical aqueous emulsion polymerization process, in system, add dispersant usually, stable with the aqueous polymer dispersion that guarantee to generate.
The dispersant that can consider comprises employed emulsifying agent and protective colloid in implementing the polymerization of free radical aqueous emulsion usually.
Suitable protective colloid for example is to gather (vinyl alcohol), cellulose derivative or comprise vinylpyrrolidone copolymers.The detailed description of relevant other suitable protective colloids can be seen in the Weyl in Houben, " organic chemistry method ", volume XIV/1, " macromolecular material ", Georg-Thieme publishing house, Stuttgart, 1969, the 411～420.Naturally, can also adopt the mixture of emulsifying agent and/or protective colloid.Employed dispersant preferably is its relative molecular weight and the protective colloid emulsifying agent that there were significant differences without exception, generally than the latter low 1000.They can be anion, cation or non-ionic.If use the mixture of surface reactive material, then nature should be compatible with each other between each composition, as this there being any query, can adopt some simple experiments to be checked.Usually, anion emulsifier is compatible with each other, and also compatible with nonionic emulsifier.
Cationic emulsifier also is the same, yet anion and cationic emulsifier are incompatible each other usually.The example of common emulsifying agent is: and one, two and trialkyl phenol of ethoxylation (the EO unit number: 3～100, alkyl: C
4～C
12), ethoxylized fatty alcohol (the EO unit number: 3～100, alkyl: C
8～C
18), and the alkali metal salt of following composition and ammonium salt: alkyl sulfate (alkyl: C
8～C
16), ethoxylated alkyl phenols (the EO unit number: 3～100, alkyl: C
4～C
12) sulfate hemiester, alkyl sulfonic acid (alkyl: C
12～C
18) and alkarylsulphonic acid (alkyl: C
9～C
18).Emulsifying agent that other are suitable such as sulfosuccinate can be seen in the Weyl in Houben, " organic chemistry method ", volume XIV/1, " macromolecular material ", Georg-Thieme publishing house, Stuttgart, 1961, the 192～208 pages.
Usually, the consumption of dispersant by the monomer weight of participating in Raolical polymerizable, is 0.5～6, preferred 1～3% (weight).
Certainly, above-mentioned dispersant generally is applicable to and stablizes handicraft product of the present invention.Yet the product of new method also comprises the aqueous dispersion of the polymer with self-emulsifying ability, and in other words, its contained polymer has ionic group, and the same sex of dependence electric charge is repelled each other and realized stabilisation.Preferably, the product of this new method itself just has anionic stabilization effect (particularly anionic dispersing agents).
If prepare to reduce the aqueous polymer dispersion of residual monomer content with mode of the present invention, be to prepare according to the monomer composition of free radical aqueous emulsion polymerisation by the monomer that includes at least one ethylenically unsaturated group, the most important thing is concerning the inventive method that then those comprise at least two kinds has the monomer of at least one ethylenically unsaturated group and remainder also comprises the monomer composition of following composition:
-70～99.9% (weight) acrylic acid and/or methacrylic acid and the ester and/or the styrene of the alkanol of 1～12 carbon atom are arranged,
Perhaps
-70～99.9% (weight) styrene and/or butadiene,
Perhaps
-70～99.9% (weight) vinyl chloride and/or vinylidene chloride,
Perhaps
-40～99.9% (weight) vinyl acetate, propionate and/or ethene,
Adding together, summation is 100% (weight).
The content of polymer solids is generally about 20～75% (weight) in suspension or the dispersion, preferred about 40～70% (weight), preferred especially 50～60% (weight).
Employed suspension or dispersion are about 10～5000 milli handkerchief seconds 25 ℃ viscosity, are preferably for 20～2000 milli handkerchief seconds, preferred especially 50～1000 milli handkerchief seconds.
Employed dispersion preferably has low viscosity.Its viscosity can be at 30～1000 milli handkerchief seconds, the preferably about 1 gram/cubic centimetre of the density of dispersion.
The definition and the assay method of relevant mensuration numerical value
Glass transition temperature
Glass transition temperature is preferably determined (G.Goldbach, " plastics, its order and performance ", " Ullmanns technology chemistry is complete works of " the 15th volume, the 219th～222 page, Weinheim, 1980) according to the specific heat in the differential thermal analysis to the dependence of temperature.
The glass transition temperature of copolymer also can be weighted by the coefficient of expansion of the mass fraction of each monomer and phase emergencing copolymer according to the glass transition temperature of concrete homopolymers and calculate to determine.
MFT
The MFT of polymer is that dispersion just still can form the minimum temperature of adhesive film after the water evaporates.This numerical value is near the glass transition temperature (H.Gerrens, " polymerization technique ", " Ullmanns technology chemistry is complete works of " the 19th volume, the 141st page, Weinheim, 1989) of polymer.
The determining instrument that uses has applied the metallic plate of thermograde above being.What observe is what temperature film to begin to occur crackle (E.Penzel, " polyacrylic acid and polymethyl acid compound ", " Ullmanns technology chemistry is complete works of " the 19th volume, the 17th～18 page, Weinheim, 1980) at.
The glass transition temperature of the acrylate that preferably uses as dispersion in this new method between-62～+ 6 ℃ (referring to E.Penzel, table 8 in " polyacrylic acid and polymethyl acid compound ", " Ullmanns technology chemistry is complete works of " the 19th volume, the 17th～18 page, Weinheim, 1980).Therefore, the polymer MFT is low more than the preferred operating temperature of the inventive method usually in the measured dispersion.So dispersion to be processed softening and easy film forming often occurs at this technological temperature.
Viscosity
Solids content is 20～75%, and is preferred 50～70%, and promptly the dispersion of this new method content range commonly used shows the wide range rheological behavior.Flow behavior depends on solids content, particle size, size distribution, and depends on the assistant system that uses in the preparation.Common observed flow abnormalities is pseudoplastic behavior and dilatancy.
Viscosity is to use capillary viscometer under the canonical measure condition, Couette viscosimeter, or (C.Gerth: " rheometry ", " Ullmanns technology chemistry is complete works of " the 19th volume, the 17th～18 page, Weinheim, 1980) of cone and plate viscometer mensuration.
The invention still further relates to the polymer dispersed preparation that reduces remaining volatile matter content with said method.
This method is particularly suitable for the shear-sensitive dispersion, as low emulsifying agent or emulsifier-free preparation, spatial stabilityization (with protective colloid or starch) dispersion or the self-dispersing system (as dispersions of polyurethanes) at thermo-responsive dispersion.
So, to implement in the device that this method is preferably described in the above, device comprises: at a) used reactor (A) of stage,, with tower (C), discharge by heat exchanger (D) at the steam of stage d) at stage c) with post-reactor (B) at stage b).Stage e) carries out in pressure-reducing station (E), stage f) in filter (F), final stage g) in former (G), carry out, this shaping stage comprises that the polymeric dispersions that will obtain is converted into the needed institute of commercial product in steps from technology.The additive that this stage may use comprises, as stabilizing agent, antioxidant, biocide, protectiveness polymer, acid, alkali, defoamer, thickener, solvent, dispersant such as water, and other suitable materials.
This new polymers dispersion preferably in sealing compound, paper and coating dispersion, whitewash in compound, jointing compound, the coating and be used as the adhesive basic material; As the basic material in paint and the coating; As adhesive or thickener, especially for interior decoration.Because remaining volatile matter content is low, this dispersion can be used for interior decoration safely, and the volatile matter of generation seldom or does not at all have, and residual remaining volatile matter is also few.
Basic material as adhesive, they can be used for for example laminated paper tinsel, as electric light, metal or the extrusion coating paper of making by copper and/or aluminium and paper, be used for the industrial layers compound, as be used in the motor vehicle manufacturing as poromerics or furniture film, as packaging adhesive, as shock resistance adhesive such as paper label and envelope, as sealing compound and ground adhesive, and be used for special coating and as adhesive.
As the paper and coating dispersion, they can be used for the surface treatment of offset printing paper, rotograyure paper and ivory board.They also can be used as the thickener of printing-ink and coating composition.
As the basic material of coating and paint, they can be used for timber paint, are used for printing industry; Be used for industrial coating such as anti-corrosion protection; Be used for emulsion enamel and emulsion paints, for example as indoor and outdoor coating, especially interior paint; The plaster and the jointing composition that are used for the interior decoration industry; As cement paint such as priming paint, house paint and concrete roof plate.
They also can be used as the coating of non-weaving cloth such as the CB coating of tufting, Nomex and mulching material or carpet, and are used for molded foam plastics and dipping goods.
Above-mentioned various uses preferably relates to indoor application, promptly uses in sealing building or compartment.
Below, will illustrate in greater detail the present invention in conjunction with example.
Example 1
Single overflow sieve-plate tower (Comparative Examples)
This tower (0.4 meter of diameter) comprises 8 single overflow sieve plates, to each other apart from 50 centimetres.Have equally distributed hole on this sieve plate, 4 millimeters in aperture.Perforated area account for plate the gross area 1.0%.Be connected with each other by the downspout that is arranged in both sides between plate and the plate.Each concrete downspout protrudes in above 40 millimeters of plate face.The dynamic pressure that steam produced like this, during operation just causes the dispersion layer of same height (40 millimeters) on the plate face.The charging of tower is: the aqueous polymer dispersion of 50% concentration, 0.2 ton/hour of flow rate is pumped to above the sieve plate of top by eccentric worm.Be upstream with charging, below the bottommost plate, introduce 40 kilograms/hour 4 crust steam.
After top plate was full of dispersion, dispersion was crossed 40 millimeters high downflow weirs and is flow to next plate along downspout, and imitative this goes on.Steam passes the perforate of bottom plate, passes the dispersion layer again, takes away the material that more and more comes out from separated dispersion in this process.After this, steam passes each piece plate more than the bottom plate by the same manner.At the cat head place, the steam that is loaded with volatile matter is drawn out of under decompression (about 200 millibars of absolute pressures) effect, and condensation in downstream condenser.Dispersion collects at the bottom of the tower of bottom plate below, delivers to the post processing station by pump at the bottom of tower.
Above experiment parameter setting value (corresponding to 1.6 cubic metres of dispersion/square metre tower sections of area load/hour) condition under, the concentration of butyl acrylate is reduced to 140ppm (plate 5) by initial concentration 415ppm.Corresponding removal efficiency is 66%, and perhaps plate efficiency reaches about 14% of thermodynamic equilibrium value.
Example 2
The single overflow sieve-plate tower
This tower (0.4 meter of diameter) comprises 8 single overflow sieve plates, to each other apart from 50 centimetres.Have equally distributed hole on this sieve plate, 4 millimeters in aperture.Perforated area account for plate the gross area 5.3%.Be connected with each other by downspout between plate and the plate.Downspout protrudes in above 100 millimeters of plate face, thereby forms downflow weir.
The charging of tower is: the dispersion that flow rate is 1500 kilograms/hour (corresponding area load be 12 cubic metres/square metre) is delivered to above the sieve plate of top.Below the bottommost plate, introduce 375 kilograms of/hour steam as the stripping medium.Pressure is 330 millibars.
In this process, the concentration of butyl acrylate is reduced to 16ppm by initial concentration 219ppm, and corresponding removal efficiency is 93%.Under each situation, the single overflow efficiency of sieve plate reaches about 11% of thermodynamic equilibrium value.
Under so high area loading condiction, plate efficiency has only reduced about 25% than Comparative Examples.Therefore, might make the tower that produces handle sufficiently high dispersion throughput, so that the effect of tower is just as the segment pipe in the whole device, and when from batch process step operational transition to continuous tower deodorization mode, do not need to establish surge tank.
Example 3
The double fluid sieve-plate tower
This tower (0.4 meter of diameter) comprises 8 double-current sieve plates, to each other apart from 50 centimetres.Sieve plate has uniform hole, 10 millimeters in aperture.Perforate accounts for 2.1% of plate area.Do not link to each other between each plate by downspout.Dispersion is passed identical hole with steam and is carried out counter current contacting.
For this reason, the charging of tower is: add 200 kilograms of/hour dispersions (corresponding area load 1.6 cubic metres/square metre hours) from cat head, and with 40 kilograms of/hour steam stripping.Pressure is 285 millibars.
In this process, the concentration of butyl acrylate is reduced to 5ppm by initial concentration 477ppm.Corresponding removal efficiency is 99%.Under each situation, double-current efficiency of sieve plate reaches about 31% of thermodynamic equilibrium value.
Find that thus this preferred double pass tray can provide removal efficiency and the plate efficiency that obviously exceeds the single overflow sieve plate.
If adopt double pass tray, the plate efficiency η that reaches depends on the throughput by the perforate cross section.(example 12) that throughput numerical value is low, efficient can be reduced to has only 7.0%.Throughput is high, and plate efficiency can be up to more than 30%, no matter pressure how (example 13～15).The aperture of single overflow sieve plate (example 4～11) is preferably 4 millimeters.Its plate efficiency is subjected to the influence of height of weir and pressure.In all tests, tower diameter is 400 millimeters.
The efficient of each time test is calculated according to formula 1,2,3,4 and 5, wherein:
m
iThe coefficient of balance of=component i (seeing formula 3)
Y
EQU=gas-liquid equilibrium concentration (% is a benchmark with the solid)
X
EQU=gas-liquid equilibrium concentration (% is a benchmark with the solid)
D=desorption factor (seeing formula 4)
N=actual plate number
n
Th=number of theoretical plate
X
aThe dispersion concentration of=outflow
X
eThe dispersion concentration of=inflow
M
St=steam flow rate, kilogram/hour
M
Disp=dispersion flow rate, kilogram/hour
α=X
a/X
e????????????(1)
η=n
th/n????????????(2)
m
i=Y
EQU/X
EQU????(3)
D=m
i*M
St/M
Disp??(4)
n
th=ln(D/α-1/α+1)/lnD-1????(5)
The deodorizing test result estimates when being standard with the concentration such as butyl propionate (α), styrene (β) and vinyl acetate (γ).Equilibrium valve m
BPrBe determined by experiment; To butyl propionate is 8.4 (concentration is benchmark with solids content in the dispersion).
Table 1: the further test of carrying out with the single overflow sieve plate
| Example | Product | Charging kg/h | Steam kg/h | Charging kg/cm 2h | Pressure mbar | ????％ | Height of weir mm | ????AL ??m 3/m 2h | Perforated area % |
| ????4 | ????α | ????1000 | ????242 | ????15.2 | ???200 | ????8.0 | ???100 | ????8.0 | ????5.24 |
| ????5 | ????α | ????1000 | ????202 | ????15.2 | ???200 | ???10.0 | ???200 | ????8.0 | ????5.24 |
| ????6 | ????α | ????1000 | ????254 | ????15.2 | ???330 | ????8.0 | ???100 | ????8.0 | ????5.24 |
| ????7 | ????α | ????1000 | ????253 | ????15.2 | ???330 | ???18.0 | ???200 | ????8.0 | ????5.24 |
| ????8 | ????α | ????1000 | ????253 | ????15.2 | ???400 | ???14.0 | ???100 | ????8.0 | ????5.24 |
| ????9 | ????α | ????1000 | ????256 | ????15.2 | ???440 | ???24.0 | ???200 | ????8.0 | ????5.24 |
| ????10 | ????α | ????1400 | ????355 | ????21.3 | ???440 | ???19.0 | ???200 | ???11.1 | ????5.24 |
| ????11 | ????γ | ????1000 | ????253 | ????15.2 | ???440 | ???22.0 | ???200 | ?????8 | ????5.24 |
Table 2: the further test of carrying out with double pass tray
| Example | Product | Charging kg/h | Steam kg/h | Charging kg/cm 2h | Pressure mbar | ????η％ | Aperture mm | ????AL ??m 3/m 2h | Perforated area % |
| ?????12 | ????α | ????1000 | ????250 | ????4.49 | ??????200 | ????7.0 | ???15 | ????8.0 | ???17.72 |
| ?????13 | ????α | ????1400 | ????353 | ???11.3 | ??????225 | ???31.5 | ???15 | ???11.1 | ????9.84 |
| ?????14 | ????α | ????1400 | ????375 | ???11.3 | ??????330 | ???35.0 | ???15 | ???11.1 | ????9.84 |
| ?????15 | ????α | ????1500 | ????377 | ???12.1 | ??????440 | ???31.9 | ???15 | ???11.9 | ????9.84 |
| ?????16 | ????β | ????1000 | ????253 | ????4.9 | ??????200 | ???17.0 | ???20 | ????8.0 | ????16.2 |
| ?????17 | ????β | ????1400 | ????357 | ????7.8 | ??????330 | ???15.0 | ???40 | ???11.1 | ????14.2 |
| ?????18 | ????γ | ????1220 | ????305 | ????6.0 | ??????200 | ???11.0 | ???20 | ????9.8 | ????16.2 |
Product α is that solids content 55%, main component are the adhesive dispersion of butyl acrylate and acrylonitrile.
Product β is solids content 50%, the viscosity paper and coating phenylethylene/butadiene dispersion of 40 milli handkerchief seconds.
Product γ is solids content 70%, the viscosity shock resistance adhesive dispersion that contains vinyl acetate of 150～900 milli handkerchief seconds.
For α, η for β, is about cinnamic about butyl propionate, and for γ, about vinyl acetate.
AL is the area load of dispersion on the plate.
Claims (12)
1. countercurrent tower that is used for reducing the remaining volatile matter content of dispersion, comprise 5～50 double pass trays and/or single overflow sieve plate, wherein the ratio perforated area of double pass tray be 2～25% and the single overflow sieve plate be 1～10%, the average opening diameter of double pass tray is 10～50 millimeters, and the average opening diameter of single overflow sieve plate is 2～10 millimeters.
2. by the desired tower of claim 1, it has in the following feature one or multinomial:
The internal diameter of-Ta is 400～2500 millimeters scopes,
-tower height is 6～25 meters scopes,
-the number of plates is in 5～50 scopes,
-distance between plates is 250～800 millimeters scopes,
-its lower region prolongs 1～3 meter, at the bottom of tower,
-upper zone tower diameter enlarges, reaching the purpose of from steam, isolating the dispersion drop by gravity,
-dispersion adds from the expansion district of tower.
3. device for preparing polymeric dispersions, the post-reactor (B) that it comprises reactor (A), may also have, as claim 1 or 2 defined towers (C), exhaust steam heat exchanger (D) and the decompressor (E) that may also have, filter (F) and after-treatment device (G).
4. by the desired device of claim 3, wherein the outlet of reactor (A) or post-reactor (B) is directly connected to the import of tower (C), and the centre is not established receiver in addition.
5. one kind by preparing the method for low remaining volatile matter content dispersion with the steam treatment dispersion in the countercurrent tower that comprises double pass tray and/or single overflow sieve plate, and wherein steam and dispersion are counter current contacting, and the tower internal pressure is 0.1～0.7 to cling to therebetween.
6. by the desired method of claim 5, wherein dispersion is a polymeric dispersions, and the tower internal pressure is adjusted to and makes tower top temperature be higher than the level that glass transition temperature of polymer and column bottom temperature are lower than the temperature that polymeric dispersions will loses stability.
7. by claim 5 or 6 desired methods, wherein employed countercurrent tower is according to claim 1 or 2 defined towers.
8. by any one desired method in the claim 5～7, it has in the following feature one or multinomial:
-Ta internal pressure is in 0.2～0.7 crust scope,
-Ta Nei temperature is 50～90 ℃ of scopes,
The area load of-plate was at 2～25 cubic metres/square metre hours
-steam utilization factor is in 10～50% scopes,
-by the dispersion feed flow rate of perforated area: to double pass tray, at 4～15 kilograms/square centimeter hours, to the single overflow sieve plate, 15～25 kilograms of/square centimeter hour scopes,
-dispersion throughput is 1～50 ton of/hour scope.
9. one kind prepares the method for hanging down remaining volatile matter content polymeric dispersions according to the following steps:
A) polymerization
B) the optional afterreaction that exists,
C) in countercurrent tower with the steam treatment dispersion,
D) need, steam discharged from countercurrent tower,
E) decompression of the polymeric dispersions that obtains by countercurrent tower,
F) filtration of polymeric dispersions,
G) moulding of polymeric dispersions,
Wherein the processing of step c) is implemented according to the method for any one definition in the claim 5～8.
10. by the desired method of claim 9, it is implemented in the defined device in claim 3 or 4.
11. a remaining volatile matter content is lower than the dispersion of 100ppm, polymeric dispersions especially, and it can be according to any one desired method preparation in the claim 5～10.
12. by the application of the desired polymeric dispersions of claim 11 aspect following: as sealing compound, paper and coating dispersion, whitewash the adhesive basic material in compound, jointing compound, the coating; Basic material as paint and coating; As adhesive or thickener, in particular for indoor purposes.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE1996121027 DE19621027A1 (en) | 1996-05-24 | 1996-05-24 | Continuous removal of monomer from aqueous suspension or dispersion |
| DE19621027.5 | 1996-05-24 | ||
| DE1997116373 DE19716373A1 (en) | 1997-04-18 | 1997-04-18 | Counterflow column, process plant and process for reducing volatiles in dispersions |
| DE19716373.4 | 1997-04-18 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1226181A true CN1226181A (en) | 1999-08-18 |
Family
ID=26026015
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97196719A Pending CN1226181A (en) | 1996-05-24 | 1997-05-22 | Column and process for deodorising dispersions |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0907393A1 (en) |
| KR (1) | KR20000015969A (en) |
| CN (1) | CN1226181A (en) |
| AU (1) | AU3091697A (en) |
| BR (1) | BR9709367A (en) |
| CO (1) | CO4990982A1 (en) |
| ID (1) | ID16979A (en) |
| TR (1) | TR199802417T2 (en) |
| WO (1) | WO1997045184A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103764240A (en) * | 2011-08-30 | 2014-04-30 | 赢创德固赛有限公司 | Method for producing a methionine salt |
| CN103764239B (en) * | 2011-08-30 | 2016-05-18 | 赢创德固赛有限公司 | The method for transformation of the methylthiopropionaldehyde of preparing from crude propylene aldehyde and thick methyl mercaptan |
| CN108654124A (en) * | 2018-05-31 | 2018-10-16 | 万华化学集团股份有限公司 | The device and method of volatile organic compounds in a kind of removing lotion |
| CN109758790A (en) * | 2017-11-09 | 2019-05-17 | 万华化学集团股份有限公司 | The apparatus and method of volatile organic compounds in a kind of removal acrylic emulsion |
| CN113234363A (en) * | 2021-05-11 | 2021-08-10 | 广东米奇涂料有限公司 | Children wall paint and preparation method thereof |
| CN115209971A (en) * | 2019-12-30 | 2022-10-18 | 韩华思路信株式会社 | Distillation apparatus and distillation method |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19847115C1 (en) * | 1998-10-13 | 2000-05-04 | Basf Ag | Counterflow stripping tube |
| DE60035141T2 (en) | 1999-02-18 | 2008-02-14 | Nippon Shokubai Co., Ltd. | Perforated bottom without drain, column with perforated bottom without drain and process for distillation |
| MY122671A (en) * | 1999-03-06 | 2006-04-29 | Basf Ag | Fractional condensation of a product gas mixture containing acrylic acid |
| DE69900030T2 (en) | 1999-06-18 | 2001-05-10 | Nat Starch Chem Invest | Removal of volatile organic compounds from polymer latices / dispersions |
| DE10109066A1 (en) * | 2001-02-24 | 2002-09-12 | Tesa Ag | Low-outgassing acrylic PSAs |
| DE102011087138A1 (en) | 2011-11-25 | 2013-05-29 | Wacker Chemie Ag | Process for the preparation of aqueous polymer dispersions |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL129660C (en) * | 1964-08-24 | |||
| JPS5813563B2 (en) * | 1976-04-03 | 1983-03-14 | 信越化学工業株式会社 | Method and apparatus for removing unreacted monomers from an aqueous dispersion of vinyl chloride |
| DE2640546C2 (en) * | 1976-09-09 | 1982-07-01 | Hoechst Ag, 6000 Frankfurt | Process for the continuous removal of vinyl chloride from an aqueous dispersion of homo- and copolymers of vinyl chloride |
| US5382390A (en) * | 1990-09-10 | 1995-01-17 | Uop | Multiple-downcomer fractionation tray with vapor directing slots and extended downcomer baffles |
-
1997
- 1997-05-22 KR KR1019980709529A patent/KR20000015969A/en not_active Application Discontinuation
- 1997-05-22 AU AU30916/97A patent/AU3091697A/en not_active Abandoned
- 1997-05-22 CN CN97196719A patent/CN1226181A/en active Pending
- 1997-05-22 EP EP97925936A patent/EP0907393A1/en not_active Withdrawn
- 1997-05-22 WO PCT/EP1997/002639 patent/WO1997045184A1/en not_active Application Discontinuation
- 1997-05-22 TR TR1998/02417T patent/TR199802417T2/en unknown
- 1997-05-22 BR BR9709367A patent/BR9709367A/en not_active Application Discontinuation
- 1997-05-23 CO CO97028494A patent/CO4990982A1/en unknown
- 1997-05-26 ID IDP971752A patent/ID16979A/en unknown
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103764240A (en) * | 2011-08-30 | 2014-04-30 | 赢创德固赛有限公司 | Method for producing a methionine salt |
| CN103764240B (en) * | 2011-08-30 | 2016-04-20 | 赢创德固赛有限公司 | Prepare the method for methionine salt |
| CN103764239B (en) * | 2011-08-30 | 2016-05-18 | 赢创德固赛有限公司 | The method for transformation of the methylthiopropionaldehyde of preparing from crude propylene aldehyde and thick methyl mercaptan |
| CN109758790A (en) * | 2017-11-09 | 2019-05-17 | 万华化学集团股份有限公司 | The apparatus and method of volatile organic compounds in a kind of removal acrylic emulsion |
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| CN108654124A (en) * | 2018-05-31 | 2018-10-16 | 万华化学集团股份有限公司 | The device and method of volatile organic compounds in a kind of removing lotion |
| CN108654124B (en) * | 2018-05-31 | 2020-11-24 | 万华化学集团股份有限公司 | Device and method for removing volatile organic compounds in emulsion |
| CN115209971A (en) * | 2019-12-30 | 2022-10-18 | 韩华思路信株式会社 | Distillation apparatus and distillation method |
| CN115209971B (en) * | 2019-12-30 | 2024-06-04 | 韩华思路信株式会社 | Distillation apparatus and distillation method |
| CN113234363A (en) * | 2021-05-11 | 2021-08-10 | 广东米奇涂料有限公司 | Children wall paint and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0907393A1 (en) | 1999-04-14 |
| BR9709367A (en) | 1999-08-10 |
| WO1997045184A1 (en) | 1997-12-04 |
| TR199802417T2 (en) | 1999-03-22 |
| CO4990982A1 (en) | 2000-12-26 |
| KR20000015969A (en) | 2000-03-25 |
| ID16979A (en) | 1997-11-27 |
| AU3091697A (en) | 1998-01-05 |
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