EP0808880A2

Silanized silicas

Abstract

Silica has a specific surface area of 80-400 m<2>/g, primary particle size of 7-40 nm, tamped density of 50-300 g/l, pH or 3-10, carbon content of 0.1-15% and dibutyl phthalate (DBP) value < 200%. Also claimed is a method of preparing silanised silica (I).

Term

Term ended

Projected expiry passed 10 April 2017, 9.5 years ago.

3 claims: 1 independent, 2 dependent

c-de-0001
Silica with the following physicochemical properties:specific surface m 2 /G 80-400 primary nm 7-40 tamped density g / l 50-300 pH 3-10 Carbon content % 0.1 to 15 DBP number % <200

16 paragraphs, as filed

p0001The invention relates to a low-thickening, silanized silica, a process for their preparation and their use.

p0002The invention relates to a silanized silica with the following physicochemical properties: <tables id="tabl0001" num="0001"><table frame="all"><tgroup cols="3" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">specific surface</entry><entry namest="col2" nameend="col2" align="left">m<sup>2</sup>/G</entry><entry namest="col3" nameend="col3" align="right">80-400</entry></row><row><entry namest="col1" nameend="col1" align="left">primary</entry><entry namest="col2" nameend="col2" align="left">nm</entry><entry namest="col3" nameend="col3" align="right">7-40</entry></row><row><entry namest="col1" nameend="col1" align="left">tamped density</entry><entry namest="col2" nameend="col2" align="left">g / l</entry><entry namest="col3" nameend="col3" align="right">50-300</entry></row><row><entry namest="col1" nameend="col1" align="left">pH</entry><entry namest="col2" nameend="col2" /><entry namest="col3" nameend="col3" align="right">3-10</entry></row><row><entry namest="col1" nameend="col1" align="left">Carbon content</entry><entry namest="col2" nameend="col2" align="left">%</entry><entry namest="col3" nameend="col3" align="right">0.1 to 15</entry></row><row><entry namest="col1" nameend="col1" align="left">DBP number</entry><entry namest="col2" nameend="col2" align="left">%</entry><entry namest="col3" nameend="col3" align="right"><200</entry></row></tbody></tgroup></table></tables>

p0003Another object of the invention is a process for the preparation of the silanised, low thickening silica, which is characterized in that a silica, in a suitable mixing vessel with intensive mixing, optionally a plurality of first with water or dilute acid and then from a surface modification or a mixture Oberflächenmodifizierungsreagentien sprayed, mixed for 15 to 30 minutes, at a temperature of 100 to 400 ° C over a period of 1 to 6 h, is tempered and then the hydrophobic silanised silica by mechanical action (for example in a ball mill) destructured / compacted and in a mill (for example, air jet mill, pin mill) nachvermahlt.

p0004As silica may preferably have a pyrogenic by way of flame hydrolysis of SiCl<sub>4</sub> produced silica can be used.

p0005As the surface may for example hexamethyldisilazane are used.

p0006Another object of the invention is the use of the inventive low thickening, silanized silicic acid for the preparation of low-viscosity polymer systems having a low yield point, such as 1- and 2-component peroxidkondensations- and addition-crosslinking silicone rubber compositions, adhesives, impression materials, sealants, etc., to their use as matting agents, for example in paints, films, as FreeFlow means (for example, SAP, fire extinguishing powder), for producing Kabelgelen, as anti-sedimentation in liquid plastic systems and reactive resins (eg synth. marble, polymer concrete, dentures) as polishing agents and / or abrasives.

p0007The inventive low-thickening, silanized silica has the following advantages:

p0008In polymer systems that are reinforced with synthetic silicas, good mechanical strength can be achieved only at very high degrees of filling. This is achieved in known silicas only by an in situ hydrophobization of the booster silica in the manufacture / compounding of appropriate sealing, casting and Dupliermassen etc. This procedure is very time and energy consuming.

p0009The silica of the invention made possible by its low thickening action and low yield point, for example, high filler loadings and therefore good mechanical strength. The above complicated compounding process can be largely eliminated.

p0010The inventive method has the advantage that due to the continuous process control reduces fluctuations in product quality occur.

example

p0011Aerosil 200 is mixed with 4.3 parts water and 18.5 parts of HMDS (hexamethyldisilazane) and annealed 140 ° C. The hydrophobic silanised silica is then compressed to a continuously operating vertical ball mill at about 250 g / l. Thereafter, the silica is re-ground using an air jet mill.

p0012The Kieseläsure obtained has the following characteristics: <tables id="tabl0002" num="0002"><table frame="all"><tgroup cols="8" colsep="1" rowsep="1"><colspec colnum="1" colname="col1" colwidth="19.68mm" /><colspec colnum="2" colname="col2" colwidth="19.68mm" /><colspec colnum="3" colname="col3" colwidth="19.68mm" /><colspec colnum="4" colname="col4" colwidth="19.68mm" /><colspec colnum="5" colname="col5" colwidth="19.68mm" /><colspec colnum="6" colname="col6" colwidth="19.68mm" /><colspec colnum="7" colname="col7" colwidth="19.68mm" /><colspec colnum="8" colname="col8" colwidth="19.68mm" /><thead valign="top"><row><entry namest="col1" nameend="col1" align="center"><b>example</b></entry><entry namest="col2" nameend="col2" align="center"><b>BET m</b><sup><b>2</b></sup><b>/G</b></entry><entry namest="col3" nameend="col3" align="center"><b>Tamped density g / l</b></entry><entry namest="col4" nameend="col4" align="center"><b>pH</b></entry><entry namest="col5" nameend="col5" align="center"><b>C content</b></entry><entry namest="col6" nameend="col6" align="center"><b>Loss on drying%</b></entry><entry namest="col7" nameend="col7" align="center"><b>Loss on ignition%</b></entry><entry namest="col8" nameend="col8" align="center"><b>DBP number%</b></entry></row></thead><tbody valign="top"><row><entry namest="col1" nameend="col1" align="left">VT 1128/1</entry><entry namest="col2" nameend="col2" align="right">145</entry><entry namest="col3" nameend="col3" align="right">188</entry><entry namest="col4" nameend="col4" align="char" char=",">7.3</entry><entry namest="col5" nameend="col5" align="char" char=",">2.7</entry><entry namest="col6" nameend="col6" align="char" char=",">2.4</entry><entry namest="col7" nameend="col7" align="char" char=",">0.3</entry><entry namest="col8" nameend="col8" align="right">90</entry></row></tbody></tgroup></table></tables>

Performance Testing

2K RTV Silicone Rubber (degree of filling 20%)

p0013<tables id="tabl0003" num="0003"><table frame="all"><tgroup cols="3" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" morerows="1" rowsep="1" align="left">rheology:</entry><entry namest="col2" nameend="col2" align="left">flow limit</entry><entry namest="col3" nameend="col3" align="left">1.9 Pa</entry></row><row><entry namest="col2" nameend="col2" align="left">viscosity</entry><entry namest="col3" nameend="col3" align="left">30,9 s<sup>-1</sup></entry></row></tbody></tgroup></table></tables><tables id="tabl0004" num="0004"><table frame="all"><tgroup cols="3" colsep="1" rowsep="0"><colspec colnum="1" colname="col1" colwidth="52.50mm" /><colspec colnum="2" colname="col2" colwidth="52.50mm" /><colspec colnum="3" colname="col3" colwidth="52.50mm" /><tbody valign="top"><row><entry namest="col1" nameend="col1" morerows="3" rowsep="1" align="left">Mechanical properties:</entry><entry namest="col2" nameend="col2" align="left">tensile strenght</entry><entry namest="col3" nameend="col3" align="left">1.7 N / mm<sup>2</sup></entry></row><row><entry namest="col2" nameend="col2" align="left">elongation</entry><entry namest="col3" nameend="col3" align="left">230%</entry></row><row><entry namest="col2" nameend="col2" align="left">Tear resistance</entry><entry namest="col3" nameend="col3" align="left">14.0 N / mm</entry></row><row><entry namest="col2" nameend="col2" align="left">Shore A hardness</entry><entry namest="col3" nameend="col3" align="left">34</entry></row></tbody></tgroup></table></tables>

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14 members in 7 offices

This recordMember, by publication datePriority claim

Priority claims4

Priority claims
Document	Office	Kind	Date
19616781	Germany	–	1996-04-26
19616781	Germany	A	1996-04-26
DE1996116781	–	–	–
19616781	–	–	–

Members14

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Document	Office	Kind
CA2203726A1	Canada	A1	1997-10-26
DE19616781A1	Germany	A1	1997-11-06
KR970069878A	Republic of Korea	A	1997-11-07
EP0808880A2This record	European Patent Office (EPO)	A2	1997-11-26
CN1167729A	China	A	1997-12-17
JPH1087317A	Japan	A	1998-04-07
US5959005A	United States of America	A	1999-09-28
EP0808880A3	European Patent Office (EPO)	A3	1999-10-27
KR100260325B1	Republic of Korea	B1	2000-07-01
CA2203726C	Canada	C	2001-08-07
CN1083397C	China	C	2002-04-24
EP0808880B1	European Patent Office (EPO)	B1	2003-01-08
DE59709069D1	Germany	D1	2003-02-13
JP3553315B2	Japan	B2	2004-08-11

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2017-07-31	Lapsed in a contracting state [announced via postgrant information from national office to epo]LapsedPG25	PG25	EP
2017-05-03	Patent expired after termination of 20 yearsExpiredPE20	PE20	GB
2017-04-19	Patent expired because of reaching the maximum lifetime of a patentExpiredMK	MK	NL
2017-04-10	Expiry of rightR071	R071	DE
2016-08-31	Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP	PGFP	EP
2016-07-29	Annual fee paid to national office [announced via postgrant information from national office to epo]GrantedPGFP	PGFP	EP
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2016-04-21	Fee paymentPLFP	PLFP	FR
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2003-08-22	Fr: translation filedET	ET	EP
2003-04-30	Gb: translation of ep patent filed (gb section 77(6)(a)/1977)GBT	GBT	EP
2003-02-13	Corresponds to:REF	REF	EP
2003-01-08	Designated contracting statesAK	AK	EP
2003-01-08	European patent grantedGrantedNOT ENGLISHFG4D	FG4D	GB
2002-11-22	(expected) grantORIGINAL CODE: 0009210GRAA	GRAA	EP
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2001-05-02	Party data changed (applicant data changed or rights of an application transferred)RAP1	RAP1	EP
2000-12-20	First examination report despatched17Q	17Q	EP
1999-11-03	Information provided on ipc code assigned before grant6C 09C 1/30 A, 6C 09C 3/12 B, 6C 09D 7/12 B, 6B 01J 2/30 B, 6C 09K 3/14 B, 6C 08K 9/06 BRIC1	RIC1	EP
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1997-11-26	Request for examination filed17P	17P	EP
1997-11-26	Designated contracting statesAK	AK	EP
1997-10-10	Public reference made under article 153(3) epc to a published international application that has entered the european phaseORIGINAL CODE: 0009012PUAI	PUAI	EP

Silanized silicas

Abstract

Term

Priority claims4

Members14

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Events

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Classification

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