Compositions of hydrocarbon-substituted diphenyl amines and high molecular weight polyethylene glycols; and the use thereof as water-tree retardants for polymers

* Background of the Invention The service life of the Isolated Power Cables is known to be shortened by an effect of water sequestration. Consequently, impregnation based on polymeric compositions, such as, for example, ethylene polymer compositions, is amenable by the addition of various additives to provide a Resistant Isolation characterized by secretion. Water excretions occur when Isolation is subjected to an electric field for a long time while they are present in an environment where water exists. These excretions are called so because they resemble branches. Indeed, water secretions are thin passages or gaps that are white in water when filled with water but become inactive when dry. For the sake of observation, specimens with water excretions must be boiled or stained with water; or irregularities, such as the interface between the Isolation and a semiconductor layer.

In the case of gaps or contamination, the secretions tend to form opposite positions of the point of tension (the nuclei) and at the same time. Both types of water-excretion ^, bound like a bow and vaporized, appear to be Archil, · Live and develop through different inequalities, as a result of their different reaction to excretion retardation that they have been exposed to ^t*

<img file="GR77987B_D0001.tif" />

<img file="GR77987B_D0002.tif" />

T.

To date, no simple retardant water-secretion system has been developed when added to a polymeric composition, resulting in a composition or having a perfectly acceptable or equilibrium properties, including dans of bow and water-excretion of the vagrant.

DESCRIPTION OF THE DRAWING

The figure is a schematic partial view showing the apparatus used to force the bogeys to develop into a test specimen.

DESCRIPTION OF THE INVENTION * The parouosa invention provides a flame ddato ekkrizooeos composition comprising a diphenyl amino substituted hydrocarbons and high molecular weight polyethylene glycol which, when added to polymeric materials such as an ethylene polymer, provides compositions which have a commercially acceptable balance of properties comprising resistance to the formation of dans bow secretions and vasodilators. The compositions of the present invention retain resistance to water-secretions over long periods of time, at normal operating temperatures or in the service of the isolated electrical conductors around any extrinsic surfaces. The present invention may be processed by flowering or water-excreting, cross-products, without significant increases in physiological concentrations of the cross-linked agent, i.e. The organic formulation by addition of a suitable diacrylate, pro, and acetate as stated. biphenyl amines, substituted moieties of one or more hydrocarbon radicals, On the Aromatic Rings, those suitable for the purposes of the present invention are acids having the formulas of

R * where each R is likely to be the same or different, is a hydrocarbon radical, being an alkyl or aralkyl substituted at the positions rather than at least one amino group.

As a rule, each R has 5-18 carbon atoms, preferably 8-9 carbon atoms. Examples of such radicals are acids derived from α-dolphins, such as n-hexene, n-heptene, n -ctene, n-nonenone, and the like as well as aryl styrene, n-heptane radicals.

Particularly desirable for the purposes of the present invention are liquid biphenyl amines, as described, being diphenyl amine acylated with acetylene or acetylene. A liquid diphenyl amine alkylated with styrene and sold under GOORYEAR TIRE AND RUBBER COMPANY under the trade name WINGSTAY 29 is an example of such a compound. of the following equiv.

<img file="GR77987B_D0003.tif" />

<img file="GR77987B_D0004.tif" />

<img file="GR77987B_D0005.tif" />

In fact, it is believed that this compound is a mixture of mildly disubstituted species.

Compositions containing a liquid hydrocarbon substituted diphenyl amine, in combination with high molecular weight polyethylene glycol, except as characterized by the properties described above, are described hereinafter, in particular.

Other suitable biphenyl amines are described hereinafter. Polyethylene glycols suitable for the purpose of the present invention are those having a molecular weight of about 100 to about 20,000.

Especially preferred polyethylene glycols have carbon numbers, i.e. carbon vapor numbers of at least 30, preferably at least 80. These materials are described in the brochure of UNION CARBIDE CORPORATION No F-4772 I, 1/78 under the heading CARBOWAX, polyethylene glycol.

A percentage of polyethylene glycol, relative to diphenyl amine, is sufficient to provide a composition or otherwise, when added to a polymeric material resulting in a polymeric composition or having an improved impermeability.

Preferably, or the amount of chlorethylene glycol, relative to the hydrocarbon substituted amine is about 0.2 to about I by weight by weight I part by weight.

C diphenyl amine. 1

Among suitable polymeric materials such as or the aforesaid retarding composition may be added to provide water-resistant compositions of ethylene polymers, as they are normally sterile. and diagonal monomers? Examples of suitable copolymerized monomers are α-olefins such as propylene, butylene-I, dxene-I and similar dienes monomers as are butadiene, isoprene and the like; polymers containing at least about 70% by weight of ethylene.

Preferred copolymers are ethylenepropylene copolymers, ethylene butene copolymers and the like. These oblique portions are capable of being produced at a low pressure of about 150 to about 300 PSI, using a modified oxide catalyst in color. .

* If desired, but polymers such as polypropylene, ethylene-propylene gum, ethylene-propylene diene gum and the like may be added to the ethylene polymer compositions of the present invention.

The compositions of the present invention may contain antioxidants such as the sterically hindered phenols and amines polymerized 2,2,4-tetramethyl hydroxyquinol, 4,4 * -thio-bis (butyl-3-methylbenzyl) (3-methylbendyl) , 5-dithydro-butyl-4-hydroxy) hydroxycinnamic acid ester of distearyl thiodipropionate, and the like.

Also, the compositions of the present invention may contain crosslinking agents when the compositions are to be used as vulcanised or crosslinked wool products as thermoplastic compositions. 3 &lt;29u, issued on 3 January 1967. i; ^;· ’ ·

These compositions may also be simply used, or

<img file="GR77987B_D0006.tif" />

Specifically desired compositions treated for the purposes of the present invention include ethylene polymers, a hydrocarbon substituted diphenyl acrylate carbamoyl polyacrylamide polyethylene amine; junction having the average type II

CH = CH, (

R^x0 j — S i — O —— ψ —— R '

I. ^CH&gt;

where Rj and Rg are both likely to be the same or different are hydrocarbon radicals having generally 6-18 carbon atoms preferably 12-14 carbon atoms, or not being integer; having a value of 4-20 preferably 4-16 ' or a silane junction promoter having the average formula I

<td></td><td>r x</td><td></td><td></td>

<td>Type III</td><td>ck = ch₂ 1</td><td></td><td>CH, 1 *</td>

<td>R^I.0-</td><td>-Si-0 ----</td><td></td><td>-Si-0—</td>

<td></td><td>I.</td><td></td><td> 1</td>

<td></td><td>CK₅</td><td>X</td><td>CHj</td>

<td></td><td>z</td><td></td><td> s</td>

where R and R₉ are as previously defined and X and ¹

Those that may be the same or different are integers with a value of 4-8.

Examples of suitable radicals for Rj and Rg are alkyl radicals such as acetyl, nonyl, decyl, indecyl, dodecyl, stearyl and the like.

Pure silane preparations within the scope of Formula II and Formula III can be prepared readily by reaction of methyl vinyl dichlorosilane or a mixture of methylvinyl dichloroilane and dimethyl dichloroides. ^. neutralization of dxinon ypoloipon.Oi molar Anal&gt; why 'g water and alMoolis MAY poikiloun relatively prys each mole of difunctional chlorosilane that the following stoichiometric equation is retained, wherein for purposes of comfort The reactants are shown that are methyl vinylchlorosilanio, ddor and dodecyl alcohols.

CH = CH₂ CI-Sl-CL + (n-I) H₂0 4 2C_I2H₂₅OH CH,

CH = CH, i '

-0-4 - SI-0—

I.

CH, ^CI2^K.25 4 ^{2nd HCL}

When preparing silane droplets for the purpose of formula III, the amount of methyl vinyl chlorosilane (X) present or the amount of dimethyl chlorosilane (Y) will be equal to or equal to the amount of the following vehicle.

CHbCH₂ CH₅

I 1

X CL-Si-CI-fY CL-Sl-CL + n-I 3 ^ 2 C_I2H₂₅OH ------&gt;

i 1

CH_:

CH-

<td></td><td></td><td></td><td></td>

<td></td><td>CH = CH₂</td><td></td><td>CH₅</td>

<td></td><td> 1</td><td></td><td> 1</td>

<td></td><td>—As — 0 ---</td><td> —</td><td>—S1-0—</td>

<td></td><td> 1</td><td></td><td> 1</td>

<td></td><td>CH,</td><td>Y -</td><td>CH,</td>

<td></td><td></td><td></td><td> - ⁵ &gt;</td>

The specificities of the reaction are shown by the methods given in detail below.

Dillane-I, characterized by gel permeation chromatography and nuclear magnetic resonance chromatography as a type

OH = βH_?

I ^ 1 ^ 25 ° $ j-0 f ^Ciep25

<img file="GR77987B_D0007.tif" />

n Ac ft?

CH:

\·»

<img file="GR77987B_D0008.tif" />

T &lt;5 silane I prepared? as follows:

* Inside a two-liter 5-neck vessel equipped with additional funnel, mechanical stirrer, thermometer and distillation head, with nitrogen diode-protected receiver, 846.0 g were added.

(6.0 g) methylvinyl dichloro silane. From the addition funnel it was added as 294.7 g. (I, 5 g) of dodecanol in the container at a gentle rate with stirring. The temperature of the vessel was lowered to 10 ° C due to HCl release. After addition of dodecanol, 89.7 g. (5.0 gram or 95% of the stoichiometric amount) of water was slowly added from the addition funnel at or above the temperature of the container maintained at +10 ° C with an external ice bath. After the addition of water, the vessel was maintained at 15.5 ° C for an additional 3 hours with stirring (HCl equilibration step). * Antibody addition funnel was purified by a K. cleaning tube₂ and the contents of the container After 30 minutes, a sample from the container was analyzed and found to contain 0.4 equivalents of 0E.^-/ gr. sample. * The constituent amount of water (4.5 g, 0.25 g) was added as saturated Ka₂C0j, solution, * Heating resumed at 30 ° C at 80 ° C, continuing to clean N₂ everywhere. The residual bicarbonate was neutralized with liquid RaHCD ^. The resulting product was filtered to yield 759.0 g. (theoretical 792.5 g) 96% of theoretical pure, colorless liquid with a viscosity of 16.5 CSTK (25 ° C) with 0.01% chloride oxide content. (0.04%).

The source of dodecanol used in the preparation of the silanes noted herein was a PROCTER and GAMBIE product Co-1214 FATTY ALCOHOL, a brand name for a mixture containing dodecanol and a small amount of alcohol. l

Silane-2 characterized by gel chromatography and nuclear magnetic resonance have the formula®¹ ·£&lt;··.'«.

- ** n Ut: * - -: / '

CH = CH₂ ) -Si-0 -----? 2^H25 ^WellP^e^ ch₅ &lt;·.

ixet

<img file="GR77987B_D0009.tif" />

^CI2^H25°

IO * 282.0 g were added to a 3-neck I-liter vessel equipped with addition funnel, condenser, mechanical stirrer, thermometer, and nitrogen passage. (2.0 grams) of methylvinyl dichlorodilane. * 98.25 g of the addition funnel was added. (0.5 grams) of dodecanol, slowly with stirring, sat or temperature was maintained between IO-I5 ° C. After addition of dodecanol, 28.4 g. (1.58 g), 90 # of the required stoichiometry of 1.75 g) of water were added with stirring, maintaining a temperature between 10 ° C and 5 ° C on the reaction medium through an ice bath. The contents of the vessel were stirred for 3 hours. The temperature between 10 ° C-5 ° C. * The addition funnel was resuspended from a tube inside the liquid reaction mixture and nitrogen passed through the mixture while warming to 90 ° C without stirring for half an hour. The vessel .- After about 0.5 h at 90 ° C or a residual amount of water (3.1 g), all residual acid chloride was then saturated, then neutralized as described for silane dilution I. 250 ° C. gr. 18.4 CSff} (25 ° C) of pure, colorless liquid was obtained.

Silane-3 characterized by gel permeation chromatography and nuclear magnetic resonance have the average formula}

Oj-gH ₂₅θCH-CH.-2α-^The~ | —C_I2H₂₅CH, 16

Silane 3 was prepared according to the method described for silane I by reaction of 282.0 g. (2 g) methyl vinyl dichlorosilane, 46.6 g (0.25 g) of dodecanol and 33.75 (1.875 g), H₂° produced ^ s ^ g. net;

colorless liquid.

Silane-4, characterized by chromatography of Sepharose.

<img file="GR77987B_D0010.tif" />

II

<img file="GR77987B_D0011.tif" />

and nuclear magnetic antiseptics have the average formula!

^CI2^H25^C

<td></td><td></td><td></td>

<td>CH, I. ³</td><td></td><td>CH »CH_OΊ ²</td>

<td>S I-0-</td><td></td><td>-Si-0 ---</td>

<td> 1</td><td></td><td> 1</td>

<td>CH₅</td><td> 4</td><td>0th₅</td>

<td>X&gt;</td><td></td><td></td>

° I2^THE25

Silane 4 was prepared according to the method of description for silane I, by reaction of 141.09 (1.0 g) methylvinyl dichlorosilane 129.1 g (ΐ, 0 g) dimethyl dichloroilane 93.29 (0.2 g). 5 d) of dodecandle and 31.5 g (ΐ, 75 g) of water to yield 193.5 g. pure colorless liquid.

In the formulation of the compositions of the present invention or the amount of high molecular weight polyethylene glycol, hydrocarbon substituted diphenyl amine, organic perpendicular and crosslinked silane promoter based on it;

* Biphenyl amine is present, together with polyethylene glycol; Of molecular weight, an amount is sufficient to improve the resistance to the water-secretion of the composition, generally in an amount of about 0, 2 to about 2% by weight, preferably about 0.5 to about 1% by weight.

High molecular weight polyethylene glycol, together with diphenyl amine, is present in an amount sufficient to improve the water-curing resistance of the composition, generally in an amount of about 0.2 to about 1% by weight, preferably about 0.2 to about 0.2. % by weight.

Organic peroxide is present in an amount sufficient to treat the composition for a cross product, generally in an amount of about 1-3% by weight, preferably in an amount of about 1.5 to 2% by weight. ^J * The cross-promoter is available in a quantity of up to

- 'o' F · V n ·:, '....

about 2% by weight, preferably about 0.5 to about 4% by weight.

It should be noted that constituent mixtures, as disclosed herein, may be used if desired. The following is a description of the materials used to carry out the examples and tests of Table I and Table II, which follow.

Description of polymers

Polymer A-ethylene and n-butene copolymer have a melt index of 0.7 and a density of 0.92.

Polymer B-polyethylene having a melt index of 2 and density

0,92 .

Very few C-polyethylene having a melt index of 0.2 and a density of 0.92.

Diphinyl amine (DPA)

I) D._jStyrene alkylated phenyl amine (WINGSTAY929 ~ e00DYEAfi TIRE AND RUBBER CO. CRANY) liquid.

II) Diisobutylene alkylated bisphenyl amine (NAUGALUBE 438L-INIR0YAL.INC) water.

III) Diphenyl amine acetylated alkyl (STALITE -RT -VANDERBILT, COMPANY) liquid

IV) Diphenyl amine alkyl methyl styrene (NAUGARD 445V)

3NIPOA1, IN0) -solid.

V) Alkylated biphenyl amine with octylene azetate-β-HT. VANDERBILT, COMPANY, INC) solid.

Description of Antioxidants (AOs)

AC-I 4,4 * -thio-bis (6-6 -butyl-3-methylphenol)

AO-2 Bistearyl thio-dipropionate ester

AO-3-Thiodiethylene-bis- (3,5-di- · 1-butyl-4-hydroxy) hydroxycinnamic ester.

<img file="GR77987B_D0012.tif" />

the

Polyethylene glycol. Polyethylene glycol-molecular weight about 40 ^) The trade name CARB0WAX under UNION CARBIDE CORP

<img file="GR77987B_D0013.tif" />

'*7^

Polyethylene glycol-weight of approximately 20,000-sold 20M under UNION CARBIDE COBPORATION.

The method used for the synthesis and testing of the compositions in Table I is described below.

Ethylene polymer alkylated biphenyl amine and polyethylene glycol glycosyl molecules were loaded into a BRABENDER stacker and combined at a melting temperature of about I50 ° C. Ventilated water-secretion-counted-water-secretion rate (WIGR) -associated conditions were determined in detail as described in USP 4,263,158 issued on or after April 21, 1981, hereinafter issued. KZZ, 5 Ki 72 h. By definition, the WIGR of a composition in which no water-soluble additive was added was 1.0 (control 6, in Table I, control A in Table II).

* Fidelity-like secretion-secretion-scintillation-stained microscope, 40x magnification, The specimens prepared as described by the WIGR test and noting the number and size of the secretions without a bow. determined by spraying samples of 1/100 thickness of an Indo, leaving the samples at room temperature for one month, by examining the surface of the specimens for secretion and quantitative estimation. From a commercial point of view, the primary purposes in this regard are for the compositions to be used as electrical impellers , which in their turn are environmentally friendly.

WIGR-too earlier or less by 0.2 fiducial binding water-secretion estimation-less AP4 blossom-low epiphytic secretion level

The examples in Table I and Table II illustrate the present invention and are not intended to limit this scope.

The blocks shown in the tables are parts by weight.

j

P »

• i

<img file="GR77987B_D0014.tif" />

<img file="GR77987B_D0015.tif" />

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<img file="GR77987B_D0017.tif" />

I.

The cross-compositions of Table II were prepared by loading the components into a BRABENBER Mixer and coupling the resulting mixture to a melt temperature of about 120 °.

D. Each composition was granulated and molded with test specimens at a temperature of I25 ° C. The test specimens were processed to a mold at a temperature of I20 ° C. Before the WIGR test, each process was performed.

<img file="GR77987B_D0018.tif" />

The tests mentioned in Table II were carried out as follows. WIGR-determined at 5 KV, I KHz, 72 hours.

<img file="GR77987B_D0019.tif" />

MONSANTO rheometer test, described in detail in USP 4,018,852 issued April 19, 1977 and referred to in pounds.

Resistance to physical degradation determined using processed specimens prepared as described above by means of an ASTMD-638 method of restraint elongation assay.

* Flowering determined by removing untreated spiked specimens to remain for one month at temperatures ranging from 7 ° C to 60 ° C, visually examining the surface of the specimens for secretion and making a sieve. Water-secretions as a cartridge bound, each molded by two-sheet molding, each 0.02 inch thick by placing a small amount of powdered; huh.

<img file="GR77987B_D0020.tif" />

mold at 180 ° C. The peroxide residues were removed by heating the test samples for seven days in a vacuum oven at a temperature of 85 ° C. Referring now to the accompanying figure, the test sample (2) was placed and maintained in the central opening of the glass vessel (4) by dividing the glass vessel (4) into two compartments. Test specimen (2) was in contact with a 0.1% normal sodium chloride solution (6) contained in a glass vessel (4) with an aqueous solution (6) connected to a voltage source (not indicated). high voltage (8) and grounded by earth wire (IC). An AC voltage-5 KV, 1 KHz was applied to the guiding line for 2 days, and after the 2-day period the sample was stained with an aqueous solution of methylene blue which made the aqueous secretions visible. , with 40X direction, and was classified qualitatively on a scale from 0 (no water-secretion without a bow binder) to 4 (many water-secretions as a bow binder).

Initial commercial purposes in relation to WIGR, 00aTO excretions such as bow tie and swelling have been described previously.

* The primary commercial purpose in relation to the degree of treatment is 48 ^ 4 pounds-Tdg * centrifugal restraint 7 days at 50 ° C, greater than 75%.

<img file="GR77987B_D0021.tif" />

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<img file="GR77987B_D0022.tif" />

Silane routers, hereinafter noted, are the subject of an application registered by HERBERT E.

PETTY, Series No ....... registered and assigned to UNION CARBIDE CORPORATION.

Melting index, as noted herein, is in milligrams per minute determined by ASTM test D-I238. The density as noted herein is in grams per cubic centimeter determined by ASTM test D-I5O5.