Process for the preparation of polymer particles

Details Process for the preparation of polymer particles Process for the preparation of polymer particles

2000-09-20

2001-10-30

Foelak, Morton (Department: 1711)

Synthetic resins or natural rubbers -- part of the class 520 ser

Synthetic resins

Cellular products or processes of preparing a cellular...

C521S082000, C521S064000

Reexamination Certificate

active

06310109

ABSTRACT:

The invention relates to a process for preparing water-expandable polystyrenes (WEPS) by polymerizing styrene in aqueous suspension, where the suspended styrene droplets comprise an emulsion of finely dispersed water.
Expandable polystyrene (EPS) beads are normally prepared by polymerizing styrene in aqueous suspension in the presence of a volatile organic blowing agent. The usual blowing agents are hydrocarbons, in particular pentane. In order to protect the environment, pentane emitted during the production and processing of EPS has to be reclaimed. This is complicated and costly. In the longer term, therefore, it would be useful to replace these organic substances with blowing agents which are less hazardous, for example water.
Eindhoven University 1997 dissertation by J. J. Crevecoeur “Water Expandable Polystyrene” describes a process for preparing WEPS by firstly preparing a fine emulsion of water in styrene with the aid of surface-active substances, polymerizing the styrene to a conversion of 50%, suspending the mixture in water with phase inversion, and finally polymerizing the styrene to completion with the aid of peroxide initiators. The surface-active substances used comprise amphiphilic emulsifiers, e.g. sodium bis(2-ethylhexyl) sulfosuccinate or sodium styrenesulfonate, or block copolymers made of polystyrene blocks and of polystyrenesulfonate blocks. All of these substances have both a hydrophilic and a hydrophobic radical and are therefore able to emulsify water in styrene.
A disadvantage of this process is that it is carried out in two stages: water is first emulsified in the styrene/polystyrene mixture and then the organic phase is suspended in water, with phase inversion.
It is an object of the present invention, therefore, to develop a simpler, single-stage process for preparing WEPS.
We have found that this object is achieved by carrying out the suspension polymerization in the presence of 5 to 30% by weight, preferably from 10 to 25% by weight, of recycled molded polystyrene foam (recycled EPS material). Recycled EPS material is obtained from treatment of EPS foams, e.g. of packaging materials or insulating materials. After the surfaces of these materials have been cleaned, the materials are comminuted, e.g. by grinding or chopping, producing flakes of foam with sizes of from 5 to 50 mm. These flakes are washed, dried, compacted and extruded to give pellets. For the novel process these pellets are then dissolved in styrene, and the solution is suspended in water and polymerized.
Pelletized EPS material generally comprises from 0.1 to 2% by weight, preferably from 0.2 to 1% by weight, of coating agents deriving from production of the EPS. These were applied to the EPS beads once they had been produced. The majority of these coating agents are amphiphilic compounds dispersed or dissolved in the styrene solution, and for the purposes of the present invention they act as emulsifying agents. Examples of coating agents are antistats, such as quaternary ammonium alkylsulfonates, aliphatic sulfonates and oxalkylated ammonium salts; anticaking agents, such as metal salts of fatty acids, e.g. zinc stearate, or else fatty esters and fatty amides; or agents for reducing cooling time, for example glycerol esters or hydrophobic esters of fatty acids or of fatty alcohols, e.g. glycerol monostearate or tristearyl citrate.
In the novel suspension polymerization it is preferable for styrene to be the only monomer used. However, up to 20% of the weight of styrene may have been replaced by other ethylenically unsaturated monomers, such as alkylstyrenes, divinylbenzene, acrylonitrile, 1,1-diphenylethene or &agr;-methylstyrene.
In the suspension polymerization the customary auxiliaries may be added, e.g. suspension stabilizers, free-radical initiators, flame retardants, chain transfer agents, expansion aids, nucleating agents or plasticizers. It is advantageous for the suspension stabilizers used to be inorganic Pickering dispersing agents, e.g. magnesium pyrophosphate or tricalcium phosphate, in combination with small amounts of alkylsulfonates. Preferred flame retardants are organic bromine compounds, e.g. hexabromocyclododecane, added in amounts of from 0.1 to 2% by weight, based on the total of styrene and recycled material.
It is appropriate for the suspension polymerization to be carried out in two temperature phases, using two peroxide initiators decomposing at different temperatures. The suspension is first heated to 80-90° C., whereupon the first peroxide, e.g. dibenzoyl peroxide, decomposes and the polymerization is initiated. The temperature is then slowly allowed to rise to 100-140° C., whereupon the second peroxide, e.g. dicumyl peroxide or di-tert-butyl perbenzoate, decomposes.
The WEPS beads obtained from the suspension polymerization comprise, depending on the amount of recycled EPS material used and on the content of coating agents, from 2 to 20% by weight, in particular from 5 to 15% by weight, of water. Their bead size is from 0.2 to 5 mm, preferably from 0.5 to 2 mm. They may be foamed using air at from 110 to 140° C., or using superheated steam, to give foam beads. A particularly elegant foaming process which gives foam beads of very low bulk density is described in the German Patent Application P 198 12 854.1.
Like conventional EPS foam beads, the WEPS foam beads can be fused to give foam sheets, foam slabs or foam moldings, used as insulating materials or packaging materials.
All percentages in the examples are by weight.


REFERENCES:
patent: 98/01489 (1998-01-01), None

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