Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.
NEW CLAIM
1. A Process for emulsion polymerization
comprising the steps:
- of reacting together a polymerization
initiator, a reductor, and a polymerizable species, with
the proviso that the polymerization initiator is not a
hydroperoxide, wherein the polymerization initiator and
the reductor are reacted together to provide a free
radical moiety of the initiator,
characterized in that the free radical moiety
initiates polymerization of the polymerizable species,
this step being carried out at an initial cold start
temperature, whereafter the temperature is actively
increased by means of an external heat supply source so
that the polymerization follows an increasing temperature
profile to a final preselected polymerization
temperature, this final temperature being higher than the
cold start temperature,
wherein the polymerization initiators are
selected from the group consisting essentially of
aliphatic and aromatic peroxy esters and peroxy
carbonates.
12a
CLAIMS
2. Process according to claim 1 carried out at an initial temperature of up to
70°C, for example carried out at an initial temperature of up to
50°C and
preferably of up to 35°C.
3. Process according to claim 1 or 2 carried out at an initial temperature
lying
in the range of +10° to 35°C, preferably in the range of
15° to 25°C.
4. Process according to any one of the preceding claims wherein the initial
temperature is maintained for a predetermined length of time, for example
up to 2 hours, preferably up to 1 hour, most preferably up to half an hour.
5. Process according to any one of the preceding claims wherein the
temperature is increased subsequent to the initial temperature
maintenance period to follow a temperature profile to a final
polymerization temperature, preferably up to a final polymerization
temperature of at the most 90°C, and wherein the final polymerization
temperature preferably lies in the range of 50-80°C and most preferably
is
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70°C or less.
6. Process according to claim 5 wherein the initial temperature is increased
incrementally per pre-selected time period, preferably by about 20°C
per
hour.
7. Process according to claim 6 wherein the initiator is selected from the
group consisting essentially of: diisobutanoyl peroxide, cumyl
peroxyneodecanoate, 2,4,4-trimethylpentyl-2-peroxyneodecanoate, tert-
amyl peroxyneodecanoate, bis(4-tert-butylcyclohexyl)peroxydicarbonate,
bis(-ethylhexyl)peroxydicarbonate, tert-butyl peroxyneodecanoate, dibutyl
peroxydicarbonate, dicetyl peroxydicarbonate, dimyristyl peroxy-
dicarbonate, tert-amyl peroxypivalate, tert-butyl peroxypivalate, bis(3,5,5-
trimethylhexanoyl) peroxide, dilauroyl peroxide, didecanoyl peroxide, 2,5"-
bis(2-ethylhexanoylperoxy)-2,5-dimethylhexane, tert-amyl peroxy-2-
ethylhexanoate, dibenzoyl peroxide, tert-butyl peroxy-2-ethylhexanoate,
tert-butyl peroxydiethylacetate, 1,4-bis(tert-butylperoxycarbo)cyclohexane,
tert-butyl peroxyisobutanoate, 1,1-bis(tert-butylperoxy)-3,3,5-
trimethylcyclohexane, 1,1-bis(tert-butylperoxy)cyclohexane, tert-butyl
peroxy-3,5-trimethylhexanoate, 2,2-bis(tert-butylperoxy)butane, tert-
butylperoxy isopropyl carbonate, tert-butylperoxy 2-ethylhexyl carbonate,
tert-butyl peroxyacetate, tert-butyl peroxybenzoate, di-tert-amyl peroxide,
dicumyl peroxide, bis(tert-butylperoxyisopropyl)benzene, 2,5-bis(tert-
butylperoxy)-2,5-dimethylhexane, tert-butyl cumyl peroxide, 2,5-bis(tert-
butylperoxy)-2,5-dimethyl-3-hexyne, and di-tert-butyl peroxide.
8. Process according to claim 7 wherein the initiator is substantially non
water-soluble and is selected from the group consisting essentially of:
- alifatic and aramatic peroxyesters, preferably tert-butyl peroxy-2-
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ethylhexanoate (Trigonox 21), tert-amyl peroxy-2-ethylhexanoate, tert-
butyl peroxybenzoate (Trigonox C), tert-amyl peroxybenzoate, tert-butyl
peroxyacetate, tert-butyl peroxy-3,5-trimethylhexanoate, tert-butyl
peroxyisobutanoate, tert-butyl peroxydiethylacetate, tert-butyl
peroxypivalate;
- peroxycarbonates, preferably tert-butyl peroxyisopropyl carbonate
(Trigonox BPIC), and tert-butyl peroxy-2-ethyl hexyl carbonate Trigonox
117).
9. Process according to any one of the preceding claims wherein the reductor
is chosen from the group consisting essentially of: sodium formaldehyde
sulfoxylate (SFS), sodium bisulfate, Ascorbic acid (vitamin C), aldehydes, for
example glutaraldehyde, sodium metabisulfite, sodium dithionate, and
sugars.
10. Process according to any one of the preceding claims wherein the
polymerizable species is selected from the group consisting essentially of:
acrylonitrile, acrylic acid, methyl acrylate, ethyl acrylate, butyl acrylate,
2-
ethylhexyl acrylate, methoxyethyl acrylate, dimethyl aminoacrylate,
methacrylic acid, methyl methacrylate, ethyl methacrylate, butyl
methacrylate, isobutyl methacrylate, 2-ethylhexyl methacrylate, lauryl
methacrylate, stearic methacrylate, dimethyl aminomethacrylate, allyl
methacrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-
hydroxyethyl methacrylate, 2-hydroxypropyl methacrylate, acrylamide,
methacrylamide, glycidyl acrylate, vinyl ester of versatic acid, styrene, para-
methyl styrene, vinyl acetate, alpha-methyl styrene.
11. Process according to any one of the preceding claims carried out in the
presence of a catalyst, said catalyst preferably being a water soluble salt
15
derived from a transition metal, and most preferably being selected from the
group consisting essentially of Fe2+, Co3+, Cu+, and Ce3+.
12. Process according to any one of the preceding claims wherein the initiator
and the reductor are provided in the following ratios 10:1 to 1:5, preferably
4:1 to 1:2.
13. Process according to any one of the preceding claims wherein the ratio of
catalyst: oxidator is about 0-0.1 on a molar basis.
14. A polymer obtainable according to the process of any one of the preceding
claims.
15. Polymer according to claim 14 having one or more of the following
characteristics:
- a conductivity lower than about 5,
- a low residual monomer level,
- a particle size of less than about 220 nm, preferably less than 200 nm.
16. Use of a polymer according to claims 14 and/or 15 in coatings and/or
adhesives.