DE1570164A1 - Process for the recovery of hydroxyethyl cellulose from film waste - Google Patents

Description

Sign in Stuttgart, the 6th time in 1965

Rayonier Incorporated P 1118 Y / W 161 Bast A2nd Street
York, MY (USA) -

Method for office glazing clay Hydroxyäthyloelluloeβ from polyethylene waste

The invention relates eich to cellulose fibers that from one with a hydrophobic layer of moisture-proofing · ■ sewn Xrager foil, and has a process to the subject after the waste of such cellulose films to recover the substances from the carrier film and the

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the hydrophobic 3ohioht forming chemicals treated The invention relates in particular to the treatment of coated foils made of an alkali-solvent

. borrowed Hydroxyäthyioellulose -träger, which is coated with a ^ zmo] ^ a "deep hydrophobic Bari"". iB a with a copolymer of vinylidene chloride and yinyl chloride or corresponding compounds

ι *

The treatment of kunetharibeeohiohteten Oelluloee-Sragerfolien sur separation of the substances of the carrier film tone the chemicals of the Sohioht was so far very much difficult and practicable and untrustworthy and ee amounts of single waste have been thrown away so far was before practical oh-not even possible, the alka-

: lilöeliohe «ydroxyfttbyloelluloee au * one bit one

thetmoplaeiieonen Han oohiohteten Polie to regain, special then «if the 8ohioht bit of the Tx * - gerfoil is bound or anchored in the foil was.

The yydjoxyätnyloelluloee the questionnaire contains nor-. ajälerweiee ea · 3 to 8>, yorsugsweiee oa. 4 pounds of attached xthylene oxide and is in a 5 pound hat ro n- ' lye Löelich. Such carrier foils are precautionary

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with a thermoplastic copolymer eue vinylidene chloride and one of the compounds vinyl chloride, acrylonitrile or methyl methaorylate is associated therewith ei · are water-repellent. Suitable «harae of this type become τοη the Dow Chemical Company under the trade - reward SABAH rert rubbed.

The German patent application R 40 179 tlb / f 5e

eohreibt an epeeiellee method sur feulslonsb · " • ohlohtung τοη Hydroiyätnyloelluloee-Trigerfolien not Such copolymers in which there is a slight adhesion de · Harsee en the carrier film is obtained. In other procedures, the trafer foil is usually used Bit in solution 8ARAtf-Polynerieat «n or ■ with a Zueaanenseteung which is in the process of being approved « in nitrocellulose as mushrooms and Wake up to the wet-foot-mowing smock will. Especially when the shoe is on the foil T-linked or anchored are very Bohwer withdraw or remove.

In contrast, the invention has an effect Procedure for separating the components of the authorized Foil and their JlUok recovery in one state created, which is suitable for the use

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net and it enables the recovered substances to be transferred directly to the original treatment solution * u ~ rUoksufWatches. This results in substantial economic wages Advantages in the production of oilulose films '' got.

The invention consists in the fact that the film waste in ' small particles are subdivided from these particles and from dilute aqueous sodium hydroxide solution Slurry is formed, this slurry is passed through a mechanical shearing device in which the slurry is crushed further y "rringert" is what * u a fast Dissolving the Hydroxyäthyloellulose in the aqueous solution leads, and that the aqueous Hydroxyätoyloellulose solution Clay is separated from the undissolved Hareteilohen.

Duroh dl · Invention is thus created sin very effective ·· process, near the waste of one made of alkali oil Hydroxyäthyloellulose existing film, which is coated with an impenetrable hair, redissolved in a lye and both the hydroxyethyl cellulose as well as the Hans in undeveloped condition can be recovered.

The invention further comprises a multi-stage process - 909833/1308

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drive, at «do the waste of the covered foil iwerst beiepielaweise with the help of a ripper or eintr Hamasermühle in Seilohen with a surohme ·· er of the above. Crushed 3 to 6.5 mm and then cut into a suitable amount of a diluted and cooled Lye, e.g., a Taigen caustic soda, soled with velvet will »Then the pollen waste will be distributed the deeies in contact with the chilled Lye can be kept in a Soherbehandluig a mechanical shearing device with high rotating speed subjugated, wofctl the poles in extremely small S) * ilohen «, the J ^ ydroxyiithyloelluloee-.Beetandtiil in the lye completely loosened and the untwisted ski material Äarin in? Orm of ex ^ mt jftinen, slightly atau- .separating Tellohen benefits.

At the aforementioned level of vision, you have to pay attention Care must be taken to ensure that no overheating occurs, since the temperature dissolved in the lye is ine tibex & external heating BjrdroxyäthyleeliulOBQ negatively influenced. He erheblioh " Eaerglesufuhr "die" around S between the foil particles and bus peeling off the Harzoohioht τοη dics «n Rope is required leads to an increase. This temperature increase should be at the

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used consentrations at a maximum of 10 Mb 30 ° C be restricted. By pre-cooling the lye to 0 to 5 ° C before the start of the heating process, you can avoid an excessively high final temperature.

In a typical implementation of erfindungsgealflen process are Poli wastes that consist aue _t roll ends Zueohneideäbfällen and others, in an amount sufficient for the moisture protection Dloke connected to a SABAN-Beeohlchtungeharz or beeohichtet are "" ersohnitsel * and * in an aqueous Jfatriumhydroxyd solution for Dissolving the X carrier film consisting of hydroxyethyloellulose is intended, see below. 11 ^ Mixture containing rubbish slurried. The sons of this AufsohlBisung are then given mechanically in "rather small ropes" and the Harmeohioht from the Sellohen Äbfeeogeu, whereby the 8onnitrfel are in contact with the lye. for example through an Oakee or Barrington mixer, at temperatures below 30 ° C and preferably below 20 ° C. The correct supply of energy and the correct degree of fragmentation by the shear effect are of great importance, since if the dimensioning is too small, the layer will not be separated from

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1670164

the carrier film and, in the case of a high dimensioning, rather a hot gelation of the material of the Srager film as a result of this dispersion and dissolution is achieved Mixer is applied to the mixture for only a few seconds. Sab ·! the non-permeable, hydrophobic thermoplastic barrelshioht remains in the solution as a finely divided solid, which can be separated by continuous centrifugation. The acquisition of both the I ^ ydroxyäthyloellu los · and the bars ·· is practical, quantitative »b.iondr» ώοή ^ τά ^ · * ^

is wendst, - dM "aseetKual ^ slioh, 3" dooh JLa "Here Aindestens 5 ^ 1 gen caustic soda Itfslioh 1st NND beiepielsweiee about 4 i discrete adipose Xthylenoxyd contains and loading with a SABAN bars or similar Ears: is coated.

The basic ideas embodied in this invention can be applied to all film waste from Hydroxyäthylotllu-

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loose, whether coated or not, are used, However, their use is particularly advantageous when the carrier film is coated with resins 'That is basically impenetrable for caustic soda and is particularly difficult to use with previous methods remove are · The inventive method can auoh for the recovery τοη Hydroxyäthyloellulose from Laminates are used that are made from alkali-oil-free * Hydroxyethyldeliulose and alkali insoluble Polyaeren, like ζ · Β · Hlyäthylen. And Polypropylen, b * «t * hen. The method according to the invention, however, does not work gan «» e * bhde ** f '* Ur HÜcVwintng a HydroxyäthyloeUulose ->? olle suitable that, as in the Deuteohen Patent application R 40 179 Vlb / 756 b * eohrleben, with

an aqueous SARAK Etaulelon let and dried by infrared radiation.

The following examples show an application of the invention Process on a Hydroxyätnylcelluloee film, with an aqueous emulsion of a Οό-polyserisates is coated from vinylidene chloride and vinyl chloride and in which the layer duroh infrared radiation heated and bonded to the carrier film.

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Example I.

Foil pellets, aB ₄ slotted roll ends, leaves, and foil sections exhibiting dimensional errors, such as occur during manufacture, were cut up on a hammer mill with sieve holes of about 6.5 mm in diameter so that the particles obtained had one size

of approximately 40 rom. It turned out that this Size too large to avoid clumping Lumps in the subsequent wet process stages' of importance 1st. 52 kg, ten-pounded polien waste, which contained about 36 kg of soluble hydroxyethyl cellulose, 417 kg of an aqueous solution containing 7 »6 percent by weight sodium hydroxide were added with this mixed well and pre-cooled to 5 ° C. Already after a few minutes des. sur ensuring an even Distribution required Mlscheno was the Slurry of undissolved particles is pumped through a continuously operating Oakes mixer, which is connected to

a peripheral speed of 12 m / 'oeo and a passage width of. 0.75 mm. Was operated, resulting in a temperature increase to 20 ° C. After a time of only 15 seconds, during which the mixture was exposed to the strong mixture, the hydroxyethyl cellulose component was completely dissolved.

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On the other hand, a 4 hour boil brought identical ones Waste chips in water are not complete Separation of the layer. Boiling in dilute acid requires 2 hours for the coating resin to separate and leads to cleavage of the Hydroxoxyäthyloelluloee. Cooking in dilute caustic soda requires more than 1 hour s; ur separation and results in a Discoloration and cleavage of the Hydroxyäthyloelluloee and Incomplete removal of the layer · Even standing in alkali for 24 hours does not lead to any problems complete dissolution of the Hydroxyäthyloelluloee, since one side of the layer adheres and prevents penetration of the lye and the hydroxyethyl oil cellulose. Hinsiohtlioh of the difficulties that arise in separating the Sohicht according to traditional methods it is surprising that the custom of the In accordance with the invention, the separation of the ohemi- ". alien to such a great extent.

After the end of the shearing and dissolving process the solution containing the insoluble layer rose was then given a dwell time of 30 seconds continuously operating centrifuge with a centrifugal force of 2000 times the force of gravity. Of the Compacted layer residue was removed from the centrifuge

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separated and collected for further processing and recovery of the layer resin. Me solution of the. recovered Hydroxyäthylcelluloae was clarified by filtration and then set for reprocessing a · * by up to an extent of 10 i "Fee it tt with a freshly prepared solution hydroxyethyl rush recovered Hydroxyäthylcellilose in endgültigenHydroxyäthylcellulose-Genalt was vermitoht. The physical properties of the resulting packaging film made of hydroxyethyloellulose are completely equivalent to those of a film made of the original hydroxyethyloellulose.

Example II

Waste of hydroxyethyloellulose consisting of roll ends, which contained 4 x accumulated "Xthylene oxide" and was coated with a hydrophobic SAEAN resin (polyvinylidene chloride-polyvinylchloride resin), was placed in a Haram bowl at low temperatures in order to avoid damage to the film by the action of heat , crushed until never a sieve with a mesh size of 6.5 am paosiert. The schnitzels were then poured into an approx. 5 ig en liatr-onleuge at 5 ° C in noble kertgs, i.e. the mixture was approx. 6%

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Hydroxyethyl Cellulose and 5 # Sodium Hydroxide * In the next step in a continuous sequence, the slurry was pumped through a high shear mixer (Oakes) at an energy input of approximately 2.3 PS / kg.min, with the temperature at 25 ° C rose. Care must be taken to keep the slurry cool, preferably at a temperature below 30 ° 0, so that optimum dissolution is achieved without heat gelation. The energy input depends on the adhesion of the layer and also on the initial temperature of the solution.A common An adequate power supply is in the range of approx. 1 to 12 PS / kg and min. This leads to a uniform hydroxyethylene cellulose solution which contains fragments of the Harzachioht in the form of finely divided individual particles and which is continuously removed by a centrifuge to remove these fragments. The solution is then filtered and mixed with freshly formed HydroxylthyIeellulose to prepare a solution for casting films, which contains 9.0 μl of hydroxyethyl cellulose and 5.6 # sodium hydroxide. The reused hydroxyethyl cellulose from the waste can amount to up to 10 Ψ of the semolina batch. A film which contains hydroxyethylcelluloae recovered from a TO Jt,

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Solution 'is poured has the same properties like a film made only from fresh Hydroxyäthyloellulose is cast, as can be seen from the determination of flexibility, impact resistance, tear strength and elongation. *

When properly adjusted, the sodium content one can Giefllösung using dea trfindungsgemäßen process at a standard mixture of 9.0 $> hydroxyethyl cellulose and 5.6 i »sodium hydroxide are made entirely from waste films. A film produced from such a solution shows no deterioration in properties compared to the films cast from a similar fresh mixture under the same conditions.

The inventive method can sum to 10ben of Hydroxyethyl cellulose waste is used, which are not coated, and also to dissolve!. 'hydroxyathyloellulose waste, which with others Resins, e.g. with polyethylene, polyisopropylene or with polyamides.

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Claims (5)

Claims 1) Process for the recovery of hydroxyethyl cellulose from waste of films coated with a hydrophobic resin, characterized in that, that the film waste is broken up into small particles, that from these ropes and thinned, aqueous sodium hydroxide solution to form a slurry, this slurry is passed through a mechanical shearing device in which the particle size is further reduced, resulting in rapid dissolution of the Hydroxyethyl cellulose in the aqueous solution leads, and that the aqueous'Hydroxyäthylcellulose-Löeung is separated from the undissolved resin parts 2) Method according to claim 1, characterized gektnnzeiohne.t, that a hydroxyethyloelulose film is treated, which is coated with a thermoplastic, hydrophobic resin that is firmly attached to the HydroxyäthylcelluloGe film connected is. 3) Method according to claim 1 or 2, characterized in that treated a hydroxyethyl cellulose film which is approx. 4 # deposited ethylene oxide 909833/130 * ORDINAL BATHROOM contains and in a Saigon aqueous Hatxlumhydroxyd-IiÖeung is soluble. ** · A) Process according to one of the preceding claims, characterized in that a hydroxyethyl cellulose film is treated which is coated with a copolymer of vinylidene chloride and a compound from the group consisting of vinyl chloride, acrylonitrile and methyl metal aorylate. 5) Method according to one of the preceding claims «, characterized by crushing the sum of the im Mash existing polymer particles an achievement in area from 1 to 12 PSAß dee pulp and per minute is expended and the temperature of the dispersion resulting from the slurry is controlled in such a way that because the Xeap «ratnr · Increase in the range of 10 to 30 ° C litgt and AaS maintaining an increase in the temperature of the dispersion the shredding to over 30 ° 0 is prevented » 909833/1306 bath