Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – Cellular products or processes of preparing a cellular...
Patent
1996-09-05
1997-07-29
Foelak, Morton
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
Cellular products or processes of preparing a cellular...
521 91, 521110, 521117, 521142, 521144, 521148, 521149, 521150, 521181, 521182, 521183, 521189, 521154, C08J 906
Patent
active
056522762
DESCRIPTION:
DESCRIPTION
BEST MODES OF CARRYING OUT THE INVENTION
Examples of the present invention are mentioned below along with a comparative example.
SYNTHESIS EXAMPLE 1
Polyoxypropylene having a number average molecular weight of 3,000 and sodium hydroxide were mixed at 60.degree. C. and then reacted with bromochloromethane added thereto, whereby the molecular weight of the polymer was increased. Next, allyl chloride was added to this and reacted at 110.degree. C. Thus, the terminal of the polymer was allyl-etherified. This was treated with aluminium silicate, and a pure, terminal-allyletherified polyoxypropylene was obtained.
The polyether had a number average molecular weight of 7,960, and the measurement of its iodine value revealed that the polyether had an olefinic group at 92% of its terminal. The viscosity of the polyether was measured with an E-type viscometer to be 140 poises at 23.degree. C.
SYNTHESIS EXAMPLES 2
Polyoxypropylene (of a triol type) having a number average molecular weight of 3,000 was allylated in the same manner as in Synthesis Example 1 but without increasing its molecular weight. The degree of allylation of the polymer was 87 %. The viscosity of the polymer was 3.5 poises at 23.degree. C.
SYNTHESIS EXAMPLE 3
A one-liter, three-neck flask equipped with a stirring rod, a three way stop-cock and a condenser was prepared. 114 g of bisphenol A, 145 g of potassium carbonate, 140 g of allyl bromide and 250 ml of acetone were put into the flask and stirred at 60.degree. C. for 12 hours. The supernatant of the resulting mixture was taken out, washed with an aqueous solution of sodium hydroxide, using a separating funnel, and then washed with water. The oily layer was dried with sodium sulfate, and the solvent was removed therefrom, using an evaporator. Thus was obtained 126 g of a pale-yellow liquid. Through its .sup.1 H-NMR, it was found that the product thus obtained is an allylated bisphenol resulting from the allyl-etherification of the OH group of bisphenol A. The yield of the product was 82% and the purity thereof was 95% or higher.
SYNTHESIS EXAMPLE 4
A one-liter, four-neck flask equipped with a stirring rod, a dropping funnel, a condenser with a three way stop-cock at its top, and a thermometer was prepared. 12.3 g of methylhydrogenpolysiloxane (KF-99, produced by Shin-etsu Chemical Co.) (200 mmols in terms of SiH group), 11.5 g of benzothiazole, 60 .mu.l of a solution of platinum-vinylsiloxane complex in xylene (5.0 .times.10.sup.-3 mmols in terms of platinum atom), and 10 ml of toluene were put into the flask. The resulting mixture was heated at 80.degree. C., and a solution of 7.0 g of propylene oxide-ethylene oxide copolymer that had been modified with a butyl group at one terminal and with an allyl group at the other terminal (20 mmols in terms of vinyl group), as dissolved in 80 ml of toluene, was dropwise added thereto through the dropping funnel over a period of 2 hours. After the addition, this was stirred still at 80.degree. C. for 2 hours. After the disappearance of the peak for the vinyl group in the reaction mixture was confirmed through .sup.1 H-NMR, the mixture was cooled. 10 g of active charcoal was added to this and stirred at room temperature for 1 hour. The resulting mixture was filtered, and the filtrate was concentrated. Thus was obtained a viscous liquid of polyether-modified methylhydrogenpolysiloxane.
SYNTHESIS EXAMPLE 5
A one-liter, four-neck flask equipped with a stirring rod, a dropping funnel, a condenser with a three way stop-cock at its top, and a thermometer was prepared. 12.3 g of methylhydrogenpolysiloxane (KF-99, produced by Shin-etsu Chemical Co.) (200 mmols in terms of SiH group), 11.5 g of benzothiazole, 60 .mu.l of a solution of platinum-vinylsiloxane complex in xylene (5.0.times.10.sup.-3 mmols in terms of platinum atom), and 10 ml of toluene were put into the flask. The resulting mixture was heated at 80.degree. C., and a solution of 80.0 g of propylene oxide-ethylene oxide copolymer that had been modified with a butyl group at one terminal and
REFERENCES:
patent: 4810728 (1989-03-01), Gross et al.
patent: 4943596 (1990-07-01), Gross et al.
Ando Hiroshi
Hamaguchi Shigeki
Ito Hiroshi
Kondo Kensuke
Nakanishi Naoaki
Foelak Morton
Kanegafuchi Chemical Industry Co. Ltd.
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