CN1257192C - Process for recovering polymer - Google Patents
Process for recovering polymer Download PDFInfo
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- CN1257192C CN1257192C CNB03123271XA CN03123271A CN1257192C CN 1257192 C CN1257192 C CN 1257192C CN B03123271X A CNB03123271X A CN B03123271XA CN 03123271 A CN03123271 A CN 03123271A CN 1257192 C CN1257192 C CN 1257192C
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- 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
- C08F6/14—Treatment of polymer emulsions
- C08F6/22—Coagulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- 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
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
- C08F279/04—Vinyl aromatic monomers and nitriles as the only monomers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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Abstract
The invention provides a method of recovering polymer particles in a granular form of a uniform size with few fine particles in the polymer containing ABS resin, ect. The method of recovering polymer comprises: the step of producing linear mixture of polymer latex with a coagulant, the diameter of which is 0.5-15 mm, by static mixer, ect., the step where the said linear mixture is added in the hot water of more than 50 DEG C, then agitated whereby the cream is solidified and granulated, and the step of separation by filtrating the coagulated polymer. The recovering polymer particles have the particle size distribution in which the particles of 0.5-4mm grain diameter is 70-95 wt.% by the weight of the total particle.
Description
Technical field
The present invention relates to from the polymer emulsion that contains ABS resin etc. that obtains with emulsion polymerization etc., reclaim the method for polymkeric substance, in more detail, relate to the method that reclaims the polymer particle that the micro mist particle is few, particle diameter is neat.
Background technology
As the method that reclaims polymkeric substance from polymer emulsion, existing method is: after the interpolation peptizer solidified it in polymer emulsion, dehydration, drying obtained pulverous polymkeric substance.In this existing method, solidifying by following of polymer emulsion undertaken, that is, and and in the coagulating pan of the hot water that is full of specified temperature (deciding the temperature of regulation according to desirable particle diameter), supply with polymer emulsion and aqueous coagulant solution, in this coagulating pan, stir.But in this method, because it is big to generate the size distribution of polymer particle of more micro mist particle, recovery, so there is following inappropriate situation: dehydration property is poor in (1) dehydration procedure after solidifying operation; (2) the micro mist particle stops up mesh in separation, drying process, and productivity reduces; (3) because the micro mist particle is missed or the loss of dispersing is big; (4) loose density is little and must need big storage; (5) must be in order to prevent the equipment of dust explosion; (6) when putting into mixing machine such as forcing machine, the micro mist particle disperses, further, forcing machine inner produce to depart from making to mix worsen, it is bad etc. to produce moulding.
Summary of the invention
The objective of the invention is to, from polymkeric substance, reclaim the polymer particle that the micro mist particle is few, particle diameter is neat.
The inventor draws following result, by mixed polymer latex and aqueous coagulant solution are obtained, make wire with regulation particle diameter at the paste mixture of normality scope, the paste mixture of this wire is stirred in hot water, by disjunction and curing, can reclaim the polymer particle that is substantially devoid of the micro mist particle.
The present invention as shown below.
1. the recovery method of polymkeric substance, it is the method that reclaims polymer particle from polymer emulsion, it is characterized in that, comprise with the mixture of polymer emulsion and peptizer make the wire of diameter 0.5～15mm molding procedure, above-mentioned wire mixture is put in the hot water, be cured and the solidifying operation, filter the separation circuit of the polymer particle solidify of disjunction by stirring.
2. the recovery method of above-mentioned 1 described polymkeric substance, wherein, the solid component concentration of said mixture is 15～40 quality %.
3. the recovery method of above-mentioned 1 described polymkeric substance, wherein, the temperature of said mixture, when the vicat softening temperature note of the polymkeric substance of recycle object is made Tm, more than (Tm-60) ℃, and, the scope below (Tm-10) ℃.
4. the recovery method of above-mentioned 1 described polymkeric substance, wherein, the usage quantity of above-mentioned peptizer with respect to above-mentioned polymkeric substance 100 mass parts, is 1～10 mass parts.
5. the recovery method of above-mentioned 1 described polymkeric substance, wherein, said mixture obtains by static mixer.
6. the recovery method of above-mentioned 1 described polymkeric substance, wherein, said mixture obtains by single shaft screw extrusion press or the multiaxis screw extrusion press more than 2.
7. the recovery method of above-mentioned 1 described polymkeric substance, wherein, the temperature of above-mentioned hot water more than (Tm-30) ℃, and, the scope below (Tm+30) ℃.
8. the recovery method of above-mentioned 1 described polymkeric substance, wherein, above-mentioned wire mixture cut into the length of regulation after, put in the hot water.
9. the recovery method of above-mentioned 1 described polymkeric substance, wherein, the polymer particle of recovery has the size distribution of the particle of particle diameter 0.5～4mm with respect to 70～95 quality % of all particles.
According to the present invention, the mixture of polymer emulsion and peptizer is made the wire of diameter 0.5～15mm, it is put in the hot water, by stirring, cut into the length of homogeneous basically, further solidify, therefore can obtain being substantially devoid of micro mist particle, the neat polymer particle of particle diameter, can reclaim.
When the solid component concentration of said mixture is 15～40 quality %, when putting into the wire mixture in the hot water, can not cause that wear is bad, can make progress to solidify operation.
In addition, the temperature of said mixture more than (Tm-60) ℃, and, during scope below (Tm-10) ℃,,, can make progress to solidify operation so when putting into the wire mixture in the hot water, can not cause that wear is bad because mixture has the viscosity of appropriateness.
The usage quantity of above-mentioned peptizer, with respect to above-mentioned polymkeric substance 100 mass parts, when being 1～10 mass parts, but high-level efficiency is carried out solidifying of polymer emulsion.
When obtaining said mixture, can obtain the mixture of good mixing state, in the operation, can high-level efficiency carry out its curing afterwards with static mixer.
In addition, when obtaining said mixture, can obtain the mixture of good mixing state, in the operation, can high-level efficiency carry out its curing afterwards by single shaft screw extrusion press or the multiaxis screw extrusion press more than 2.
The temperature of above-mentioned hot water is more than (Tm-30) ℃, and during scope below (Tm+30) ℃, but high-level efficiency is carried out solidifying of polymer emulsion.
After above-mentioned wire mixture cut into the length of regulation, when putting in the hot water, can obtain the more neat polymer particle of particle diameter.
According to the present invention, can improve the dehydration property of the dewatering operation in the separation circuit, prevent that mesh from stopping up, and reduces the loss of polymkeric substance.Further, by increasing the loose density of the polymer particle that reclaims, can dwindle storage.In addition, need be in order not prevent the equipment of dust explosion, when shapers such as forcing machine drop into, the micro mist particle does not disperse, so can prevent because the moulding that the segregation of the micro mist particle in the shaper causes is bad.
Below, the present invention is specifically described.
The present invention is the method that reclaims polymer particle from polymer emulsion, it is characterized in that, comprise with the mixture of polymer emulsion and peptizer make the wire of diameter 0.5～15mm molding procedure, above-mentioned wire mixture is put in the hot water, be cured and the solidifying operation, filter the separation circuit of the polymer particle solidify of disjunction by stirring.
Polymkeric substance applicatory has (i) acrylonitrile-butadiene-styrene resin (ABS resin), acrylonitrile-butadiene-alpha-methyl styrene resin (heat-resisting ABS resin), acrylonitrile-butadiene-N-phenylmaleimide resin (heat-resisting ABS resin), vinyl cyanide-ethene among the present invention, propylene, diene-styrene resin (AES resin), methyl methacrylate-butadiene-styrene are resin (MBS resin), high-impact polystyrene resin (HIPS resin), acrylonitrile-acrylate-styrene resin resinous polymers such as graft copolymer such as (AAS resin); (ii) rubbery copolymers such as styrene butadiene rubbers (SBR), acrylonitrile-butadiene rubber (NBR), acrylic rubber; (iii) acrylic resin, polystyrene, vinylbenzene-methyl methacrylate (MS resin), styrene-acrylonitrile copolymer hard resin shaped polymers such as (AS resins) etc.
Above-mentioned polymer emulsion obtains with emulsion polymerization, and solid component concentration is 20～50 quality % usually.On the one hand, as above-mentioned peptizer, be now to be used for the peptizer that polymer emulsion solidifies always, mineral acids such as hydrochloric acid, sulfuric acid, nitric acid are for example arranged, organic acids such as acetic acid, formic acid, citric acid, the metal-salt that these are sour.As these metal-salts, inorganic salt such as calcium chloride, aluminum chloride, Tai-Ace S 150, sal epsom are for example arranged, organic salts such as calcium acetate, Burow Solution.These metal-salts can directly use solid, also can make it be dissolved in middle uses such as water.
The addition of above-mentioned peptizer is considered the condensation value of the solid component concentration and the polymkeric substance of polymer emulsion, preferably with respect to 1～10 mass parts of polymkeric substance 100 mass parts, and more preferably 1～5 mass parts.When the addition of above-mentioned peptizer is less than 1 mass parts, polymer emulsion is fully solidified.On the other hand, when surpassing 10 mass parts, useless because surpass the necessary amount of peptizer.Here, above-mentioned " condensation value " is meant the polymer emulsion and the peptizer with different solid component concentrations that mixes the solid component concentration with regulation, generates sedimentary minimum temperature (mixed temperature) when generating through confirming precipitation behind the certain hour.
The method of mixed polymer latex and peptizer has no particular limits, can enumerate, polymer emulsion and peptizer are added blending means in the mixing machine respectively, and the blending means that drops into peptizer in polymer emulsion drops into the blending means of polymer emulsion etc. in peptizer.According to these methods, can be preferably formed paste.Mixing condition also has no particular limits, and considers that preferably the vicat softening temperature of the polymkeric substance of recycle object is selected temperature.When the vicat softening temperature note of the polymkeric substance of this recycle object is made Tm, the temperature during mixing preferred (Tm-60) ℃～(Tm-10) ℃, more preferably (Tm-55) ℃～(Tm-15) ℃, the scope of further preferred (Tm-50) ℃～(Tm-20) ℃.If this temperature by solidifying operation, is separated into micropartical ℃ lower than (Tm-60) in coagulating pan, the micro mist particle becomes many in the polymer particle of recovery, and it is big that size distribution becomes.On the other hand, if ℃ higher, has the tendency of the viscosity increased of mixture than (Tm-10).For at said temperature, polymer emulsion and peptizer can be heated in advance, also can add Hot mixer.Preferably the said mixture that obtains is also maintained said temperature.
The mixing machine that uses during as mixed polymer latex and peptizer has no particular limits, and can lift static mixer, single shaft screw extrusion press or the multiaxis screw extrusion press more than 2 etc.Among the present invention,, preferably use static mixer, single shaft screw extrusion press or the multiaxis screw extrusion press more than 2 as above-mentioned mixing machine.These mixing machines can endwaysly be placed, and also can place sidewards.During with the endways placement of mixing machine,, the mixture of extruding from mixing machine directly can be put into the coagulating pan by Position Design coagulating pan in the below of the outlet side (lower end side) of mixing machine.Mixing machine when horizontal, is needed in addition for this mixture being imported the equipment in coagulating pan.Use as mixing machine under the situation of screw extrusion press, from mixed performance and the viewpoint of extruding stability, 2 screw extrusion presss of preferred engagement type.
Here, the static mixer as an example of above-mentioned mixing machine is directly to connect a plurality of mixing machines unit to constitute.
The proterties of the unitary tube of each mixing machine section for example is circular, but is not limited to this, also can be ellipse, polygon etc.In order to mix continuously polymer emulsion and the peptizer that is pressed into pump etc., the mixture of generation is moved in tube, to reverse be necessary to the next door in the tube along with the tube direction.The angle that this reverses promptly, in the angle of an end face of unitary from mixing machine to next door rotation the other end, for example be 90 degree, 180 degree etc., but the angles beyond these also can.In addition, the end face cross connection in the next door of the end face in the next door of the unitary outlet side of mixing machine of leading portion and the unitary inlet side of its next section mixing machine.
The solid component concentration of the mixture that constitutes by polymer emulsion and peptizer, preferred 15～40 quality %, more preferably 20～40 quality % select the scope of preferred 25～35 quality % of a step.The solid component concentration of said mixture does not form paste and forms pulpous state than 15 quality % after a little while, is difficult to obtain the wire mixture, and the micro mist particle becomes many in the polymer particle of recovery, and it is big that size distribution becomes.On the other hand, when surpassing 40 quality %, has the tendency of the viscosity increased of mixture, so be difficult to obtain the wire mixture of diameter 0.5～15mm sometimes.
The paste mixture that constitutes by polymer emulsion and peptizer in the above-mentioned mixing machine from the outlet side that is arranged on mixing machine, extrude circle or the oval-shaped hole usually, make diameter 0.5～15mm, preferred 0.5～10mm, the more preferably wire mixture (molding procedure) of 1～5mm.So-called " diameter " is meant the wide significance of the maximum length that comprises external diameter.
This wire mixture can be a successive, also can cut into the length of regulation when extruding.Under the situation of the length that cuts into regulation, the preferred 1～10mm of its length, preferred 1～5mm.Cutting-off method has no particular limits, and the method for using stapling machine, the method for using the fluid cutting machine etc. are arranged.In addition, in the moment that the wire mixture is extruded, its temperature is the temperature when the mixing of the polymer emulsion of above-mentioned explanation and peptizer preferably.
Then, above-mentioned wire mixture is put in the hot water (water of heating) in the coagulating pan, stirred (solidifying operation).Can with this wire mixture with put in the hot water after air contacts, also can extrude and put in the hot water.
The temperature of above-mentioned hot water preferred (Tm-30) ℃～(Tm+30) ℃, more preferably (Tm-20) ℃～(Tm+20) ℃, the scope of further preferred (Tm-10) ℃～(Tm+10) ℃.If this temperature is ℃ lower than (Tm-30), and the wire mixture does not solidify at the state that drops into, and is dispersed into micropartical in coagulating pan, has the tendency that the micro mist particle increases in the polymer particle of recovery.The coagulating pan of the identical or different hot water of multistage temperature also can directly be set.At this moment, preferably make the temperature height of the hot water in the coagulating pan of back segment.Like this, because the curing of wire mixture is slowly carried out, the micro mist particle further tails off, and obtains the neat polymer particle of particle diameter easily.
Above-mentioned hot water also can be the hot water that contains peptizer or coagulant aids.
Above-mentioned present situation mixture solidifies (solidifying) in putting into hot water, further stirs, and soon with regard to disjunction, forms short-term shape or granular.Agitation condition has no particular limits.As with the agitating wing that mixes, be broken into short-term shape or granular as long as above-mentioned wire mixture can be divided efficiently in hot water, just have no particular limits.For example, can use agitating wings such as paddle, Off ァ ゥ De ラ one wing, the turbine wing, the ズ Le マ one ジ Application wing, the マ ッ Network ス ズ レ Application De wing, the Off Le ゾ one Application wing.
Obtain the polymer particle by the above-mentioned operation of solidifying, after use strainer etc. filters (separation circuit), dehydration, dry, recovery.The situation that filtration is also arranged and dewater and carry out simultaneously.
As the filtration means, belt filter, vacuum belt filter etc.As the dehydration means, centrifuge etc. is arranged.In addition, as dry means, pneumatic drier, fluidized drying machine, rotary drier etc. are arranged.Drying temperature (being called gas flow temperature) is generally (Tm-50) ℃～Tm ℃, preferred (Tm-40) ℃～(Tm-10) ℃.Polymkeric substance is ABS when being resin, preferred 50～100 ℃ of drying temperature, more preferably 70～95 ℃.
According to the present invention, the polymer particle of recovery has the following particle of particle diameter 0.5mm with respect to all, below the preferred 20 quality %, and more preferably below the 15 quality %, the further following size distribution of preferred 10 quality %.In addition, surpass the particle of particle diameter 0.5mm, more than the preferred 80 quality %, more preferably more than the 90 quality %.Further, the particle of the scope of particle diameter 0.5～4mm, with respect to all, preferred 70～95 quality %, more preferably 75～95 quality %, further preferred 80～92 quality %.The particle that particle diameter 0.1mm is following is with respect to all, below the preferred 1 quality %, more preferably below the 0.5 quality %.
The simple declaration of accompanying drawing
Fig. 1 is the mode chart of an example of the formation of expression polymer recovery device.
Fig. 2 is the explanatory view of formation of the mixed cell of expression static mixer.
Fig. 3 is other the mode chart of formation of polymer recovery device of expression.
Fig. 4 is the mode chart of the formation of the used polymer recovery device of expression embodiment 1.
Embodiment
Below, the present invention will be described to utilize accompanying drawing.
Fig. 1 represents the mode chart of an example of the formation of polymer recovery device.This retrieving arrangement has and will connect 5 sections unitary static mixers of mixing machine with the mixing machine 10 of vertical direction design, the coagulating pan (the 1st coagulating pan) 20 of input hot water.Further, at the back segment of the 1st coagulating pan 20, wet crushing mill 30, the 2nd coagulating pan 20a etc. can be set in order, water extracter 40, drying machine 50 etc.
(among Fig. 1,21a represents the turning axle of agitating wing, and 22a represents agitating wing for wet crushing mill 30 and the 2nd coagulating pan 20a.) can omit, also can further set up as required.That is, concentrate on desirable size in order to make the wire miscellany 100 of from mixing machine 10, extruding formation, can be in first coagulating pan 20 fully disjunction, under curable their situation, also can omit wet crushing mill 30 and/or the 2nd coagulating pan 20a.In addition, by slowly above-mentioned wire miscellany being cured, fully reduce the micro mist particle, wish to make under the big or small homogeneous of polymer particle, the consistent situation, design wet crushing mill 30 and/or the 2nd coagulating pan 20a also can design multistage as required.Among Fig. 1, static mixer constitutes by connecting 5 sections mixing machine unit, but is not limited to this.As long as energy thorough mixing polymer latex and peptizer can be below 4 sections, also more than 6 sections.
Constitute each mixing machine unit of static mixer, as shown in Figure 2, it is circular tubular that profile forms section, is equipped with in tube and will be split into 2 through the mixture of polymer emulsion in this and peptizer, and guiding forms spiral helicine 1 next door 12.This next door 12 is designed to the tube direction with reversing, so that can form spirrillum through the mixture of polymer emulsion in the tube and peptizer.This windup-degree, that is, the windup-degree from the end face (end face of inlet side) of tube to the next door 12 other end (end face of outlet side) is 180 degree in the example of Fig. 2.That is to say, be designed to reverse half-turn to the end face of outlet side from the end face of inlet side.This windup-degree is not limited to 180 degree, for example, also can be 90 degree, 270 degree, 360 degree etc., and the angle beyond these angles also can.In order to represent the appearance of slowly reversing in next door 12, the end face 12i in the next door of inlet side has been shown among Fig. 2 (X), the cut-out end face 12c in the next door of tube central part has been shown in Fig. 2 (Y), the end face 12o in the next door of outlet side has been shown among Fig. 2 (Z).
Each mixing machine unit makes next door 12 cross connections at leading portion and its back segment.That is, the next door end face of the unitary inlet side of mixing machine of the next door end face of the unitary outlet side of mixing machine of leading portion and its back segment forms cross one another position relation and links.Therefore, split into the polymer emulsion of 2 processes and the mixture of peptizer in the mixing machine unit with leading portion and further split into 2 when flowing into the mixing machine of back segment, its result splits into 4 constantly at this.Below, along with via the unitary hop count of mixing machine, divide fluxion to increase, can mix fully.
In the example of Fig. 2, the unitary next door 12 of each mixing machine is 1 tabular component that forms curve form, therefore, have and the mixture of polymer emulsion and peptizer is split into 2 effect, but may not need 1, for example also can be form the mixture have polymer emulsion and peptizer be split into 3 effect shape member (with the cut-out end face of tube axle orthogonal to extend to the member of the shape of 3 directions at radial direction from tube axle equal angles).In addition, also can be member with the shape that is split into the effect more than 4 (with the cut-out end face of tube axle orthogonal to extend to the member of the shape of 4 directions at radial direction from tube axle equal angles).
In addition, for the temperature that makes the mixture that forms by polymer emulsion and peptizer in above-mentioned preferable range, also can in static mixer, be equipped with heating source.
The mixture that the above-mentioned practice obtains is extruded into wire from the hole (each internal diameter is the hole about 0.5～15mm) of the majority of the punch die 11 of the lower end of mixing machine 10.
Drop into hot water in the coagulating pan 20 of input wire mixture 100.The temperature of this hot water preferred (Tm-30) ℃～(Tm+30) ℃.In this hot water, also can add peptizer or coagulant aids in advance.Coagulating pan also can design the multistage more than 2 sections as shown in Figure 1, at this moment, be set at lower temperature by temperature with the hot water of the 1st coagulating pan 20, be set in higher temperature at back segment, can slowly carry out the curing of wire mixture, the micro mist particle further reduces, and can reclaim the little polymer particle of size distribution.
In the coagulating pan 20, not shown, designed by the motivating force that will come from drive source (motor) agitating wing 22 via the rotation of turning axle 21 conduction.By the rotation of this agitating wing 22, the wire mixture of putting into the hot water of coagulating pan 20 from mixing machine 10 is broken into short-term shape or granular by branch.
Fig. 3 is the mode chart of the formation of the expression polymer recovery device different with Fig. 1.In this retrieving arrangement,, use screw extrusion press as mixing machine 10a.Other constitute because identical with Fig. 1, with identical symbolic representation, omission are described.
Used screw extrusion press is 1 in the polymer recovery device of Fig. 3, and it is institute's example, also can use the screw extrusion press of the multiaxis more than 2.When using 2 screw extrusion presss, from mixed performance and extrude the viewpoint of stability, preferred engagement type.
Embodiment
Below, enumerate embodiment the present invention is specifically described.In embodiment and the comparative example, when part and % are not specifically noted, be weight basis.
1. embodiment 1
Use contains the ABS resin (solid component concentration 35%) and the peptizer magnesium sulfate solution (solid component concentration 10%) of 90 ℃ of vicat softening temperatures, with the polymer recovery device of formation shown in Figure 4, reclaims the ABS resin particle.That is,,, reclaim polymer particle by using the polymer recovery device of static mixer as mixing machine.
In addition, the polymer recovery device that uses among this embodiment 1 is said in the strictness, and is different aspect following with polymer recovery device shown in Figure 4.That is be different on 4 sections these one side, in the mixing machine unit.Internal diameter as the static mixer of mixing machine 10 is 8mm, and the number in the hole of the punch die 11 of the outlet side design of static mixer is 3, and the diameter in each hole is 6mm.
At first, above-mentioned latex and above-mentioned peptizer respectively with 30 liters of/hour speed with 2.1 liters/hour (being equivalent to relative 100 parts in the polymkeric substance that is contained in the latex, the usage quantity that sal epsom is 2 parts), are put in the static mixer, 50 ℃ of mixing., the mixture that obtain from the punch die of the outlet side setting of static mixer be extruded into wire mixture (solid component concentration 33.4%, temperature 50 ℃), put in the hot water (90 ℃ of temperature) in the coagulating pan 20 with agitating wing thereafter.Then, in this coagulating pan 20, with revolution 120rpm rotation agitating wing, average retention time is 0.5 hour.By such stirring, confirm that the wire mixture is by disjunction.Then, filter the polymer particle that solidifies,, reclaim, measure the size distribution of polymer particle 80 ℃ of dryings.The results are shown in table 1.
2. embodiment 2
Use latex and peptizer among the embodiment 1,, reclaim the ABS resin particle with the polymer recovery device of formation shown in Figure 3.That is, as mixing machine 10a, the polymer recovery device of 2 screw extrusion presss by adopting vertical placement reclaims polymer particle.
In addition, the polymer recovery device that uses among this embodiment 2 is said in the strictness, with polymer recovery device shown in Figure 3 following 2 different.That is, do not have the 2nd coagulating pan 20a in (1), (2) screw extrusion press is 2 of engagement types, goes up different at 2.The screw diameter of screw extrusion press is 25mm, and the L/D of screw rod is 4 (L is 10cm), 50 of the numbers in the hole of the punch die 11 that is provided with at the screw extrusion press outlet side, and the diameter in each hole is 2mm.
At first, above-mentioned latex and above-mentioned peptizer respectively with 30 liters of/hour speed with 2.1 liters/hour (being equivalent to relative 100 parts in the polymkeric substance that is contained in the latex, the usage quantity that sal epsom is 2 parts), are put in the screw extrusion press, 50 ℃ of mixing., the mixture that obtain from the punch die of the outlet side setting of screw extrusion press be extruded into wire mixture (solid component concentration 33.4%, temperature 50 ℃), put in the hot water (90 ℃ of temperature) in the coagulating pan 20 with agitating wing thereafter.Then, in this coagulating pan 20, with revolution 120rpm rotation agitating wing, average retention time is 0.5 hour.By such stirring, confirm that the wire mixture is by disjunction.Then, filter the polymer particle that solidifies, reclaim, measure the size distribution of polymer particle.The results are shown in table 1.
3. comparative example
Use latex and peptizer among the embodiment 1,, reclaim the ABS resin particle with existing known retrieving arrangement.That is, the polymer recovery device by not using mixing machine 10 to constitute among Fig. 4 reclaims polymer particle.
Above-mentioned latex, above-mentioned peptizer and water (30 ℃ of temperature) (are equivalent to relative 100 parts in the polymkeric substance that is contained in the latex with 30 liters/hour, 2.1 liters/hour respectively, the usage quantity that sal epsom is 2 parts) and 9.9 liters/hour speed, do not mix and just put into (90 ℃ of temperature) in the coagulating pan 20, with revolution 120rpm rotation agitating wing, average retention time is 0.5 hour, and latex is solidified.Then, filter the polymer particle that solidifies, reclaim, measure the size distribution of polymer particle.The results are shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Comparative example | |
| More than the 4mm | 8.0％ | 1.0％ | 0.0％ |
| 1～4mm | 55.0％ | 64.0％ | 15.0％ |
| 0.5～1mm | 30.0％ | 26.0％ | 20.0％ |
| 0.1～0.5mm | 6.8％ | 8.9％ | 32.0％ |
| 0.1mm below | 0.2％ | 0.1％ | 33.0％ |
As can be seen from Table 1, in the comparative example 1, the following particle of 0.5mm has generated 65%, and wherein, the following micro mist particle of 0.1mm contains 33%.On the other hand, almost do not have the following micro mist particle of 0.1mm among embodiment 1 and the embodiment 2, the particle of other 0.5～4mm is respectively 85% and 90%.Therefore, according to the present invention, it is few to reclaim the micro mist particle, the polymer particle that particle diameter is neat.
Claims (9)
1, the recovery method of polymkeric substance, it is the method that reclaims polymer particle from polymer emulsion, it is characterized in that, comprise following operation: with the mixture of polymer emulsion and peptizer make the wire of diameter 0.515mm molding procedure, above-mentioned wire mixture is dropped in the hot water, be cured and the solidifying operation, filter the separation circuit of the polymer particle solidify of disjunction by stirring, the solid component concentration of said mixture is 15～40 quality %.
2, the recovery method of the described polymkeric substance of claim 1, wherein, the solid component concentration of polymer emulsion is 20～50 quality %.
3, the recovery method of the described polymkeric substance of claim 1, wherein, the temperature of said mixture, when the vicat softening temperature note of the polymkeric substance of recycle object is made Tm, more than (Tm-60) ℃, and the scope below (Tm-10) ℃.
4, the recovery method of the described polymkeric substance of claim 1, wherein, the usage quantity of above-mentioned peptizer with respect to above-mentioned polymkeric substance 100 mass parts, is 1～10 mass parts.
5, the recovery method of the described polymkeric substance of claim 1, wherein, said mixture makes by static mixer.
6, the recovery method of the described polymkeric substance of claim 1, wherein, said mixture makes by single shaft screw extrusion press or the multiaxis screw extrusion press more than 2.
7, the recovery method of the described polymkeric substance of claim 1, wherein, the temperature of above-mentioned hot water is more than (Tm-30) ℃, and the scope below (Tm+30) ℃.
8, the recovery method of the described polymkeric substance of claim 1, wherein, above-mentioned wire mixture cut into the length of regulation after, put in the hot water.
9, the recovery method of the described polymkeric substance of claim 1, wherein, the particle that the polymer particle of recovery has particle diameter 0.5～4mm is the size distribution of 70～95 quality % with respect to all particles.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002127464A JP3987755B2 (en) | 2002-04-26 | 2002-04-26 | Polymer recovery method |
| JP127464/2002 | 2002-04-26 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1453297A CN1453297A (en) | 2003-11-05 |
| CN1257192C true CN1257192C (en) | 2006-05-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB03123271XA Expired - Fee Related CN1257192C (en) | 2002-04-26 | 2003-04-25 | Process for recovering polymer |
Country Status (3)
| Country | Link |
|---|---|
| JP (1) | JP3987755B2 (en) |
| KR (1) | KR100984614B1 (en) |
| CN (1) | CN1257192C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4676216B2 (en) * | 2005-02-15 | 2011-04-27 | 日本エイアンドエル株式会社 | Polymer recovery method from polymer latex |
| JP4673085B2 (en) * | 2005-02-28 | 2011-04-20 | 日本エイアンドエル株式会社 | Polymer recovery method and polymer recovery apparatus from polymer latex |
| JP5138909B2 (en) * | 2006-08-18 | 2013-02-06 | 日本エイアンドエル株式会社 | Resin composition, impact resistance modifier and thermoplastic resin composition |
| JP4980676B2 (en) * | 2006-08-28 | 2012-07-18 | 日本エイアンドエル株式会社 | Polymer recovery method |
| CN102311610B (en) * | 2011-07-06 | 2012-09-05 | 惠州市昌亿科技股份有限公司 | Acrylonitrile-butadiene-styrene (ABS) composite material used for housing of intelligent water meter and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60163933A (en) * | 1984-02-03 | 1985-08-26 | Japan Synthetic Rubber Co Ltd | Recovery of polymer |
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2002
- 2002-04-26 JP JP2002127464A patent/JP3987755B2/en not_active Expired - Fee Related
-
2003
- 2003-04-25 KR KR1020030026203A patent/KR100984614B1/en active IP Right Grant
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Also Published As
| Publication number | Publication date |
|---|---|
| JP2003321547A (en) | 2003-11-14 |
| JP3987755B2 (en) | 2007-10-10 |
| CN1453297A (en) | 2003-11-05 |
| KR20030084742A (en) | 2003-11-01 |
| KR100984614B1 (en) | 2010-09-30 |
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