Silicone gel composition

 

(57) Abstract:

Silicone gel composition comprises, by weight.h.: polyorganosiloxane with an average in the molecule of the vinyl groups associated with the silicon atom, equal 3-12, (POS-1) 100, polyorganosiloxane (CSOs) 0.5 to 10, polyorganosiloxane with integral trimethylsilylpropyne with an average in the molecule of the vinyl groups associated with the silicon atom, equal 1-2, (POS-2) 20-200, platinum catalyst (in terms of platinum) 7-100 ppm. The composition has improved stability and improved performance in industrial production. 1 C.p. f-crystals, 3 tables.

The invention relates to the field of compositions based on liquid silicone rubbers cured by polyaddition reactions, and more specifically to the field of low-modulus compositions, silicone gels.

Silicone gels (KG) recently found a wide application in various industries and science, in particular, to protect the various electronic units and components from shock and vibration, as well as to create a dynamic optical models of solids.

One of the first publications devoted primeneniyu.).

Most fully in theory, the properties of the gels were investigated P. De amounts of frozen in the book "the Idea of scaling in polymer physics" (1982).

The world's leading company for the production of silicon materials produced quite a wide range KG for various purposes. In particular, the firm Tochiba KG produces under the brand name YE 5818 RTV, TSE 3051, Dow Corning brand Sylgard 527, X3-6779, Hipec 6110, the company Shin Etsu - KE 104LTV etc.

The closest technical solution chosen for the prototype is a silicone gel composition for protection of electronic components (application 63-35654, Japan, MKI C 08 L 83/05, R.J. chemistry, Ref. 2 T).

The composition contains

A) polyorganosiloxane viscosity of 50 to 10000 (300 - 5000) cSt at 25oC with an average in a molecule of H atoms associated with Si, 1, and the remaining organic groups associated with the Si atom, represent a (UN)substituted monovalent hydrocarbon radicals containing no aliphatic unsaturated groups;

B) polyorganosiloxane with the average number of vinyl groups in the molecule associated with Si, 2, and the number of the vinyl groups on the hydrogen atom A associated with Si is 0.1 to 3;

C) a catalyst based on Pt, Pd or Rh, and the content of KATALITIChESKIE protective coating on top of the hybrid structure and large-scale integrated circuits.

However, the change in the elastic modulus KG concentration of crosslinking agent - polyorganosiloxane adopted for the prototype composition has a pretty sharp dependence, i.e. small changes in the concentration of crosslinking agent leads to a significant change in the elastic modulus. This, as well as have always a place of technological variation in components of the composition lead to the fact that the modulus of elasticity KG varies from batch to batch. In some industries, for example in dynamic optical models and others, this is unacceptable.

The technical object of the present invention is to improve the stability of the compositions and their characteristics in industrial production.

The technical result is achieved by the fact that the proposed silicone gel composition includes polyorganosiloxane with integral trimethylsilylpropyne with the average number of vinyl groups in the molecule associated with Si, 3-12 (POS-1), polyorganosiloxane (CSOs) and the platinum catalyst and differs from the known presence of additional polyorganosiloxane with integral trimethylsilylpropyne with the average number of vinyl groups in the molecule associated with Si, 1-is negotiationson (CSOs) - 0,5 - 10

Polyorganosiloxane (PIC-2) - 20 - 200

The platinum catalyst (in terms of platinum) - 7 - 100 ppm.

In addition, the composition may contain oligoorganosiloxanes with integral trimethylsilylpropyne in an amount of 5 to 150 wt.h. on 100 wt.h. POS-1

The chemical composition of polyorganosiloxanes may be represented by the General formula

PIC-1 M' M150-670M3-12M',

PIC-2 M' M150-670M1-2M',

where M' - (CH3)3SiO-

M -(CH3)2SiO-; (C6H5)(CH3)SiO-; (CF3CH2CH2)(CH3)SiO-

M" - -(CH3) (CH2-CH) SiO-

The viscosity of the POS 1 and POS 2 is 200 - 6500 SST, the content of unsaturated groups, characterized by a bromine number (b h) - 3.5 to 4.5 and 0.5 to 1.5, respectively.

Get them by known methods: anionic or cationic copolymerization of cyclic and/or linear organosiloxanes. The viscosity is regulated by the dosage of lexaorganizer.exe or organosiloxanes with integral triorganosilylalka. As a catalyst for copolymerization use aqueous KOH, CsOH, (CH3)4NOH and their siloxanes, cation exchange resin, an acidic clay. Receiving POS 1 and POS 2 is illustrated by the following examples.

4, dimethylcyclohexane), 15,98 of methylphenylsiloxane (A3), 2,53 g methylvinylsiloxane (4), 1,60 g hexamethyldisiloxane (HMDS), heated under stirring to 60oC, add 2 g of cation exchanger KU-23 and keep stirring at this temperature for 4 hours. Then cation exchange resin is filtered off and distilled unreacted monomers from the resulting polymer at a temperature of 150 - 170oC and a residual pressure of 5 - 25 mm RT. Art.

Characteristics obtained in examples 1 to 8 samples are shown in table. 1.

Example 2. The process is conducted similarly to example 1, except for copolymerization take 100 g of D4, of 1.94 g of the hydrolyzate of methylphenyldichlorosilane (MSDHS), 1.4 g oligomerisation liquid PMS-1,5.

Hydrolysis MVTHS carried out as follows. In chetyrehosnuju flask equipped with stirrer, reflux condenser, dropping funnel and thermometer, download 300 ml of water and from the dropping funnel for 2 hours was added dropwise 141 g (1 mol) MVTHS, maintaining the temperature of the hydrolysis of 15 - 20oC. and Then stirred the reaction mass for another 2 hours. Separating the hydrolysate, washed until neutral, dried over calcium chloride and sodium bicarbonate and use in copolymerization 2, only for copolymerization take 100 g dimethylsiloxane liquid PMS-100, 2.6 g of the hydrolyzate MVTHS and 1.5 g of PMS in 1.5.

Example 4. In a three-neck flask is charged with 100 g of D4, 2.4 g4, with 21.4 g of methyl-cryptosporidiosis (F3), 0.75 g PMS-5, is heated with stirring to 140oC and injected into the reaction mixture 0,009 ml of 40% aqueous solution of CsOH, after 1 hour, enter 0,018 ml silentspace containing 10% H3PO4. Distilled unreacted monomers at 140 - 160oC and a residual pressure of 10 - 30 mm RT. Art.

Example 5. Analogously to example 4, only take 100 g of PMS-200, 21 g F3, 0.65 g4and 1.4 g PMS-1.5 and copolymerization are 6 hours.

Example 6. Analogously to example 1, except that as minilateral component use cohydrolysis clear (DMDS), methylphenyldichlorosilane (MSDHS) and trimethylchlorosilane (TMCS) in a molar ratio of 9 : 3 : 2.

Corydalis are as follows. In chetyrehosnuju flask equipped with stirrer, thermometer, reflux condenser and addition funnel, pour 320 ml of water. From the dropping funnel was added dropwise to water for 2 hours a mixture of 116 g DMDS, 42,3 g MVTHS and 21.7 g TMDS. Temperature cohydrolysis not exceeding 30oC. For okongo with sodium bicarbonate solution until neutral, dried over calcium chloride. The resulting cohydrolysis has a bromine number of 44.2.

For copolymerization take 100 g of D4, 15.9 g A3, 3,34 g cohydrolysis with bromine number 44.2 and 1.7 g HMDS.

Example 7. In a three-neck flask equipped with stirrer, thermometer and reflux condenser, load 100 g depolymerised D4, 1.5 g of cohydrolysis with bromine number 44,2 (see example 6) and 0.6 g of PMS is 1.5. Heat up the contents with stirring to 140oC add 0.005 g of KOH in the form of siloxanes potassium and lead the process for 1 hour, then reduce temperature to 120oC add 0.005 g H3PO4, stirred for 0.5 hours. Then distilled monomers at a temperature of 140 - 170oC and a residual pressure of 5 - 25 mm RT. Art.

Example 8. Analogously to example 1, only take 100 g of PMS-1000, 3.0 g of cohydrolysis with bromine number 44,2 (see example 6) DMDS, MSDHS, TMHS. Properties of the obtained oligomers, the viscosity and the bromine number is shown in table 1.

As cross-linking component is used polyorganosiloxane with hydrogen (HSi= 0,42 of 1.8%, with a viscosity of 10 to 130 cSt/20oC the General formula

M'

where M' - (CH3)3SiO-;

M*- CH3HSi-;

M"' - (CH3)2SiO-;

M"" - C

Example 9. In chetyrehosnuju flask (hydrolyser), equipped with a stirrer, reflux condenser with gas outlet tube and a thermometer, download 400 ml of water. A mixture of 21.7 g of trimethylchlorosilane (TMCS), 61,9 g methyldichlorosilane (MDHS), 103,2 g DMDS was added dropwise with stirring from a dropping funnel over 2 hours. The temperature of the hydrolysis of < 20oC. At the end of prebyvania the mixture is stirred for 2 hours, allow to settle for 2 hours, separate cohydrolysis, washed until neutral solution of soda, dry calcium chloride. Characteristics of the obtained dimethylethylenediamine are shown in table 2.

Example 10. The process is carried out analogously to example 9, only cohydrolysis take 5,4 g TMHS, 86,3 g MDHS, 90,3 g DMDS, and 29.9 g MPDGS. Neutral hydrolysate 105 g load in trekhgornyy flask equipped with a stirrer and a thermometer, heated to 75oC, add 2 g of resin KU-23 and lead the catalytic rearrangement for 1 hour, then filtered resin KU-23, distilled volatile at 120oC and a residual pressure of 20 mm RT. Art.

Example 11. The process is carried out analogously to example 10, only for Somer 12. The process is carried out analogously to example 10, only cohydrolysis take 2.17 g TMHS, 63,25 g MDHS, 77,4 g DMDS.

Example 13. As a cross-linking agent is used industrially produced GKZ-94 (GOST 10834-76).

Example 14. As a cross-linking agent is used industrially produced GKZ-94M (TL6-02694-72).

Properties of the obtained oligoorganosiloxanes are shown in table 2.

The composition may further contain oligoaniline (CCA), which you can use oligoaniline PMS-200, PMS-1000, 133-79, 161-44.

For the preparation of compositions components are mixed in the proportions (table 3), after which the samples utverjdayut at a temperature of 150oC for 5 hours.

The modulus of elasticity utverzhdenii composition was determined by the method which was based on the method of determining the hardness of plastics, in which the load and depth of penetration of a spherical indenter is determined by the modulus of elasticity. The depth of penetration h of the spherical indenter in the flat surface of the sample according to this theory, is

,

where E1E2,1,2the young's moduli and Poisson's ratio of the indenter and the

If E1> E2the modulus of elasticity of the material under investigation can be calculated by the depth of penetration of the indenter:

.

In examples 6 used oligomethylsiloxanes brand 133-79, 8 oligomer--cryptosporidiosis brand 161-44, 7 and 10 oligomethylsilicones with PMS 200 PMS-1000, respectively.

In the composition of the used catalysts, which represents a complex platinum compounds in which the ligands are organosilicon compounds of General formula

[(CH3)n(CH2=CH)3-nSi]2O,

where n = 0 to 2,

(US 3775452 A, 1973), and platinum on various media, etc.

Examples 11 and 12 made according to the prototype. It is seen that by increasing the concentration of crosslinking agent 2 times the modulus of elasticity is growing more than four times, while the same change in the concentration of crosslinking agent in examples 1 and 9, is performed according to the proposed formula, the modulus of elasticity increased less than 1.5 times.

Thus, the proposed arrangement provides a more gradual change in the elastic modulus of the composition change of concentration of crosslinking agent.

1. Silicone gel composition in inilah groups, associated with the silicon atom is 3 - 12 (POS-1), polyorganosiloxane (CSOs) and the platinum catalyst, characterized in that it further comprises polyorganosiloxane with integral trimethylsilylpropyne with an average in the molecule of the vinyl groups associated with the silicon atom, is equal to 1 - 2 (PIC-2), in the following ratio, wt.h.:

Polyorganosiloxane (POS-1) - 100

Polyorganosiloxane (PSO) is 0.5 - 10

Polyorganosiloxane (PIC-2) - 20 - 200

The platinum catalyst (in terms of platinum) - 7 - 100 ppm

2. Silicone gel composition on p. 1. characterized in that it further comprises oligoorganosiloxanes with integral trimethylsilylpropyne in an amount of 5 to 150 wt.h. on 100 wt.h. polyorganosiloxane (PIC-1).

 

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