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US4289860A Expired / Lapsed US ⏱️ 0.0 years remaining

Grafting of silane on thermoplastics or elastomers for purposes of cross linking

Assignee: Kabelmetal Electro GmbH
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Filing: 1975-03-10
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Granted: 1981-09-15
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Expires: 1995-03-10
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Abstract

Abstract Granulated polyethylene is agitated and mixed with a solution of silane with peroxide, activators and anti-oxidants and at a temperature between 80° to 100° C. to obtain diffusion of these additives into the polyethylene particles which is followed by grafting through extrusion or radiation which in turn is followed by exposure to and/or development of water to obtain cross-linking. A catalyst is added preferably by mixing polyethylene powder with the catalyst and adding that powder to the powder with diffused silane, after that diffusion has been completed.

Inventors

  • 👤 Fritz Glander
  • 👤 Hermann U. Voigt

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 23:12
CPC Classifications
C; C08; C08J; C08J3/00; C08J3/24; C08F; C08F230/00; C08F230/04; C08F230/08; C08F230/085; C08F291/00; C08F291/02; C08J3/20; C08J3/203

Claims Analysis

Total Claims: 38
Claim 1
Independent Claim 146 words
In a method for cross-linking thermoplastic or elastomeric material wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitating; adding a silane compound to the material prior to completion of the agitation, the silane compound being of the variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite melting range, between 80° C. and 100° C., so that the silane or silane compound as agitated together with the said material fluid is caused to diffuse into the fluid particles without grafting; and providing for grafting of the silane or silane compound molecules to the molecules of the thermoplastic or elastomeric material.
Claim 2
Dependent Claim 146 words
In a method for cross-linking thermoplastic or elastomeric material wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitating; adding a silane compound to the material prior to completion of the agitation, the silane compound being of the variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite melting range, between 80° C. and 100° C., so that the silane or silane compound as agitated together with the said material fluid is caused to diffuse into the fluid particles without grafting; and providing for grafting of the silane or silane compound molecules to the molecules of the thermoplastic or elastomeric material.
Claim 3
Dependent Claim 25 words
In a method as in claim 1, wherein the silane compound is added at a temperature below the crystallite melting range of the said powder.
Claim 4
Dependent Claim 20 words
In a method as in claim 1, wherein the silane is added at a temperature between 60° and 100° C.
Claim 5
Dependent Claim 17 words
In a method as in claim 1, wherein the grafting occurs with mechanical-thermal treatment of the powder.
Claim 6
Dependent Claim 21 words
In a method as in claim 4, wherein said treatment is carried out at a temperature between 160° and 250° C.
Claim 7
Dependent Claim 12 words
In a method as in claim 4, wherein the powder is extruded.
Claim 8
Dependent Claim 147 words
In a method for cross-linking thermoplastic or elastomeric material, wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as a dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitation; adding a silane compound to the material prior to completion of the agitation, the silane compound being of a variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite's melting range, so that the silane or silane compound, as agitated, together with the said material fluid is caused to diffuse into the fluid particles without grafting; and subjecting the material to a high energy radiation for grafting the silane or silane compound molecules upon the molecules of the thermoplastic or elastomeric material.
Claim 9
Dependent Claim 147 words
In a method for cross-linking thermoplastic or elastomeric material, wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as a dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitation; adding a silane compound to the material prior to completion of the agitation, the silane compound being of a variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite's melting range, so that the silane or silane compound, as agitated, together with the said material fluid is caused to diffuse into the fluid particles without grafting; and subjecting the material to a high energy radiation for grafting the silane or silane compound molecules upon the molecules of the thermoplastic or elastomeric material.
Claim 10
Dependent Claim 19 words
In a method as in claim 7 wherein the material has a temperature below 180° C. during said radiation.
Claim 11
Dependent Claim 19 words
In a method as in claim 1 wherein the silane compound is added to the powder prior to agitation.
Claim 12
Dependent Claim 152 words
In a method for cross-linking thermoplastic or elastomeric material, wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as a dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitation; adding a silane compound when the temperature of the powder has risen to 60° C. to 100° C. prior to completion of the agitation, the silane compound being of a variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite's melting range, so that the silane or silane compound, as agitated, together with the said material fluid is caused to diffuse into the fluid particles without grafting; and providing for grafting of the silane or silane compound molecules on the molecules of the thermoplastic or elastomeric material.
Claim 13
Dependent Claim 152 words
In a method for cross-linking thermoplastic or elastomeric material, wherein cross-linking is preceded by grafting of silane and is carried out in the presence of moistures, the combination of steps comprising: providing the thermoplastic or elastomeric material as a dry, fluid powder; agitating the powder to obtain fluidization thereof and raising the temperature by operation of the agitation; adding a silane compound when the temperature of the powder has risen to 60° C. to 100° C. prior to completion of the agitation, the silane compound being of a variety that permits grafting on the molecules of said powder; providing for a temperature below the crystallite's melting range, so that the silane or silane compound, as agitated, together with the said material fluid is caused to diffuse into the fluid particles without grafting; and providing for grafting of the silane or silane compound molecules on the molecules of the thermoplastic or elastomeric material.
Claim 14
Dependent Claim 27 words
In a method as in claim 1 or 10 wherein the silane compound is added when the temperature of the powder has risen to 80° to 90°.
Claim 15
Dependent Claim 17 words
In a method as in claim 1, and including pre-drying the powder before adding the silane compound.
Claim 16
Dependent Claim 24 words
In a method as in claim 1, wherein the silane compound is added to the powder under conditions of low pressure to obtain evaporation.
Claim 17
Dependent Claim 25 words
In a method as in claim 13, wherein the diffusion occurs from the liquidous as well as from the gaseous phase of the silane compound.
Claim 18
Dependent Claim 20 words
In a method as in claim 1, wherein the mixture is formed and subsequently placed in intimate contact with water.
Claim 19
Dependent Claim 19 words
In a method as in claim 15, and including adding to the water a substance which reduces surface tension.
Claim 20
Dependent Claim 15 words
In a method as in claim 1, wherein the silane compound is mixed with peroxide.
Claim 21
Dependent Claim 17 words
In a method as in claim 17, wherein the silane compound is additionally mixed with an activator.
Claim 22
Dependent Claim 17 words
In a method as in claim 17, wherein the silane compound is additionally mixed with an anti-oxidant.
Claim 23
Dependent Claim 19 words
In a method as in claim 1, wherein a condensation catalyst is added to the mixture subsequent to diffusion.
Claim 24
Dependent Claim 19 words
In a method as in claim 20, wherein the condensation catalyst is added under temporary continuation of the agitation.
Claim 25
Dependent Claim 25 words
In a method as in claim 20, wherein the mixture is extruded, the catalyst being added to the hot mixture as it is being extruded.
Claim 26
Dependent Claim 21 words
In a method as in claim 20, wherein the mixture is applied to an elongated object, the catalyst being sprayed on.
Claim 27
Dependent Claim 38 words
In a method as in claim 20, wherein a batch of the powder and of the catalyst is prepared to obtain diffusion of the catalyst into the latter powder and adding the batch as mixed to the mixture.
Claim 28
Dependent Claim 16 words
In a method as in claim 1, wherein the silane compound is mixed with a anti-oxidant.
Claim 29
Dependent Claim 19 words
In a method as in claim 25, wherein the oxidant is a monomer or oligomer of the 2,2,4 trimethyl-dihydroquinoline.
Claim 30
Dependent Claim 16 words
In a method as in claim 25, wherein the oxidant is also grafted onto the polymer.
Claim 31
Dependent Claim 30 words
In a method as in claim 1, wherein 0.05 to 0.5 parts per 100 parts (by weight) of powder, of a peroxide is added to the silane as solution therein.
Claim 32
Dependent Claim 13 words
In a method as in claim 28, wherein the peroxide is an ester-peroxide.
Claim 33
Dependent Claim 12 words
In a method as in claim 29, wherein the esteroxide is tert.-butylperoxy-isonanoate.
Claim 34
Dependent Claim 20 words
In a method as in claim 28, wherein the peroxide is a blend of 1, 3 bis(tert.-butylperoxy-isopropy) benzene and tert.-butylperoxy-3,3,5-trimethylhexanoate.
Claim 35
Dependent Claim 12 words
Method as in claim 1, wherein the silane compound is vinyltriacetoxy silane.
Claim 36
Dependent Claim 19 words
Method as in claim 1, wherein the fluid is higher molecular polyethylene with a melting index of about 2.
Claim 37
Dependent Claim 15 words
Method as in claim 1, and including mixing the fluidizable polymer with higher condendated substances.
Claim 38
Dependent Claim 31 words
Method as in claim 1, and including mixing the fluidizable polymer with ethylene propylene terpolymer elastomer or ethylene-propylene elastomer at 5 to 20 parts by weight per 100 parts fluidizable polymer.

References Cited (Backward Citations)

US3646155A Cited
US3830872A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1984-09-14 1985-03-16 1985-09-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1988-09-14 1989-03-16 1989-09-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1992-09-14 1993-03-16 1993-09-15 $7700.00 Window Closed / Lapsed

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