Treated fillers and uses thereof

Patent metadata

Field	Value
Publication number	US-10113111-B2
Application number	US-201514828892-A
Country	US
Kind code	B2
Filing date	Aug 18, 2015
Priority date	Feb 6, 2015
Publication date	Oct 30, 2018
Grant date	Oct 30, 2018

Abstract

The various embodiments of the present invention relate to condensation curable silicone compositions comprising: a condensation curable polyorganosiloxane; and treated particles comprising a particulate solid having an effective amount of nitrogen-containing base (e.g., a nitrogen-containing superbase) disposed thereon. Other embodiments of the present invention relate to methods for preparing the aforementioned treated particles; the treated particles themselves; and methods of using the treated particles and compositions of the various embodiments of the present invention.

First claim

What is claimed is:

1. A condensation curable silicone composition comprising:
a condensation curable polyorganosiloxane; and
treated particles comprising a particulate solid having an effective amount of nitrogen-containing superbase disposed thereon;
wherein the effective amount of nitrogen-containing superbase disposed on the particulate solid is sufficient to neutralize a substantial number of a plurality of acidic sites on the particulate solid and a substantial number of the acidic sites on the particulate solid are neutralized with the disposed nitrogen-containing superbase.

2. The condensation curable silicone composition of claim 1 , wherein the effective amount of nitrogen-containing superbase disposed on the particulate solid is sufficient so that the time necessary for the condensation curable silicone composition to cure and reach a tan delta value equal to 1 is from about 30 seconds to about 1 hour at 150° C.

3. The condensation curable silicone composition of claim 1 , wherein the particulate solid is a particulate phosphor.

4. The condensation curable silicone composition of claim 3 , wherein the particulate phosphor comprises at least one of a cerium-doped phosphor, aluminate phosphor, a silicate phosphor, a garnet phosphor, and a nitride phosphor.

5. The condensation curable composition of claim 1 wherein the nitrogen-containing superbase is a cycloaliphatic imines of the general formula:

wherein X is CH 2 or NR, wherein R is hydrogen, alkyl or aryl; and subscript n is an integer from 1 to 3.

6. The condensation curable silicone composition of claim 1 , wherein the nitrogen-containing superbase is at least one of:
1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU);
1,5,7-Triazabicyclo[4.4.0]dec-5-ene (TBD);
1,5-Diazabicyclo[4.3.0]-5-nonene (DBN); and
7-Methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene (MTBD).

7. The condensation curable silicone composition of claim 1 further comprising a catalytically effective amount of a condensation catalyst, wherein the total amount of the nitrogen-containing base disposed on the particulate solid of the treated particles plus the catalytically effective amount of a condensation catalyst disposed in the condensation curable silicone composition is such that the time necessary for the condensation curable silicone composition to cure and reach a tan delta value=1 is at least 30 seconds, but not so much that the time is greater than 65 minutes at 150° C.

8. The condensation curable silicone composition of claim 1 wherein the nitrogen-containing superbase also functions as a condensation catalyst.

9. The condensation curable silicone composition of claim 1 , wherein the condensation curable polyorganosiloxane comprises an organosiloxane block copolymer comprising:
0 to 10 mole percent M constituent units of the formula [R 3 SiO 1/2 ],
40 to 90 mole percent D constituent units of the formula [R 2 SiO 2/2 ],
10 to 60 mole percent T constituent units of the formula [RSiO 3/2 ], and
0.5 to 35 mole percent silicon bonded hydroxy (SiOH);
wherein:
the sum of the mole percent M, D, and T constituent units is 100 mole percent;
each R is independently a C 1 to C 30 hydrocarbyl;
the D constituent units [R 2 SiO 2/2 ] are arranged in linear blocks having an average of from 50 to 300 D constituent units [R 2 SiO 2/2 ] per linear block;
the T constituent units [RSiO 3/2 ] are arranged in non-linear blocks having a block weight of at least 500 g/mole;
the M constituent units [R 3 SiO1/2] are connected to T units;
at least 30% of the non-linear blocks are crosslinked with each other;
each linear block is linked to at least one non-linear block via —Si—O—Si— linkages; and
the organosiloxane block copolymer has a weight average molecular weight of at least 20,000 g/mole.

10. A cured product of condensation curing the condensation curable silicone composition of claim 1 .

11. A method for treating particulate solid having a plurality of acidic sites, the method comprising:
contacting the particulate solid with a nitrogen-containing superbase to give treated particles having an excess amount of nitrogen-containing superbase disposed thereon, wherein the amount of nitrogen-containing superbase is disposed on the particulate solid and is sufficient to neutralize a substantial number of a plurality of acidic sites on the particulate solid wherein the particulate solid is a particulate phosphor and the treated particles are treated phosphor particles.

12. The method of claim 11 further comprising:
isolating the treated particles having an excess amount of nitrogen-containing superbase disposed thereon to give isolated treated particles having an excess amount of nitrogen-containing superbase disposed thereon;
processing the isolated treated particles having an excess amount of nitrogen-containing superbase disposed thereon to remove therefrom a portion, but not all, of disposed nitrogen-containing superbase to give processed treated particles having an effective amount of nitrogen-containing base disposed thereon;
wherein the processing comprises heating the isolated treated particles having an excess amount of nitrogen-containing superbase disposed thereon at a temperature and for a time sufficient to remove therefrom the portion, but not all, of disposed nitrogen-containing superbase to give processed treated particles such that the time necessary for a condensation curable silicone composition comprising the processed treated particles having an amount of nitrogen-containing superbase disposed thereon to cure and reach a tan delta value equal to 1 is from about 30 seconds to about 1 hour at 150° C.

13. A method for treating a curable polyorganosiloxane particle-containing composition, the method comprising:
treating a composition comprising the condensation curable polyorganosiloxane and untreated particles with a solution comprising a solvent and a nitrogen-containing superbase in an effective amount sufficient to neutralize a substantial number of a plurality of acidic sites on the untreated particles;
wherein the solution comprising the nitrogen-containing superbase does not substantially dissolve the condensation curable polyorganosiloxane.

14. Treated phosphor particles comprising a particulate phosphor having an effective amount of nitrogen-containing superbase disposed thereon; wherein the effective amount of nitrogen-containing superbase disposed on the particulate phosphor is sufficient to neutralize a substantial number of a plurality of acidic sites on the particulate phosphor and a substantial number of the acidic sites on the particulate phosphor are neutralized with the disposed nitrogen-containing superbase; and wherein the nitrogen-containing superbase is a cycloaliphatic imines of the general formula:

wherein X is CH 2 or NR, wherein R is hydrogen, alkyl or aryl; and subscript n is an integer from 1 to 3.

15. The treated phosphor particles of claim 14 , wherein the nitrogen-containing superbase is at least one of:
1,8-Diazabicyclo[5.4.0]undec-7-ene (DBU);
1,5,7-Triazabicyclo[4.4.0]dec-5-ene (TBD);
1,5-Diazabicyclo[4.3.0]-5-nonene (DBN); and
7-Methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene (MTBD).

16. The treated phosphor particles of claim 14 wherein the treated phosphor particles are in the form of an isolated powder.

17. The treated phosphor particles of claim 14 wherein the tre

Assignees

• Dow Corning
• Dow Silicones Corp

Inventors

• Liu Lizhi
• Swier Steven
• Wei Yanhu

Classifications

• C09K11/02

  Use of particular materials as binders, particle coatings or suspension media therefor · CPC title

• C09C3/08

  Treatment with low-molecular-weight {non-polymer} organic compounds {(C09C3/006, C09C3/048 take precedence)} · CPC title

• C09C1/3669

  Treatment with low-molecular organic compounds · CPC title

• C08G77/44

  containing only polysiloxane sequences · CPC title

• C08G77/08

  characterised by the catalysts used · CPC title