• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 引用文献
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  • 优先权
    • 专利摘要:
    1489819 Polymer foam coated articles UPJOHN CO 4 June 1975 [9 July 1974] 24089/75 Addition to 1489820 Heading B2E [Also in Division C3] Masonite, building board, gypsum board, asbestos board (transite), wood, plywood, sheet metal and paper products e.g. Kraft paper and cardboard may be coated by spraying thereon a polymer spray foam formulation comprising (a) an aromatic polyisocyanate, (b) a minor amount of polyol. (c) a blowing agent, and (d) a catalyst mixture for trimerizing said polyisocyanate comprising per equivalent of polyisocyanate (i) 0.002 to 0.0315 equivalents of N. N-dimethvlcyclohexylamine. and (ii) 0.0055-0.022 equivalents of a tetra-(C 1 -C 8 alkyl) ammonium C 1 -C 8 -alkanoic acid salt, the major recurring polymer unit in the foam produced being isocyanurate. In the Examples spray foams prepared from polymethylene polyphenyl polyisocyanate. a silicone surfactant, trichlorofluoromethane as blowing agent, tris (#-chloropropyl) phosphate as fire-retardant agent, a polyester prepared from chlorendic anhydride, diethylene glycol and propylene oxide, optionally a polyether, N, N-dimethylcyclohexylamine and tetramethyl ammonium 2-ethylhexanoate in ethylene glycol are applied to cardboard, sheet steel and asbestos board.
    公开号:SU718014A3
    申请号:SU752153415
    申请日:1975-07-09
    公开日:1980-02-25
    发明作者:Джон Локвуд Роберт；Хейтвей Роесс Ричард
    申请人:Дзе Апджон Компани (Фирма)；
    IPC主号:
    专利说明:

    FOAM RECOVERY
    (54) METHOD
    WITH ISOCIANURATE STRUCTURE
    This invention relates to isocyanurate structured neoplasts, which can be used as insulating materials for high-temperature pipelines, furnaces, and storage tanks for liquids at elevated temperatures. They also find applications for cooling, where thermal insulation of pipelines or tanks for storing liquids at low temperatures is required.
    Due to their high heat and fire resistant properties, they can also be used in the manufacture of various structures in industrial construction.
    A known method for producing an foam with an isocyanurate structure by cyclotrimerization of an aromatic plylio gypsy ha in the presence of a polyol, a foaming agent and a mixture of N, N-dimethylcyclohexylamine and a salt of a saturated carboxylic acid. As a salt of a saturated carboxylic acid, an alkali metal salt of 1 is used.
    However, the foam obtained by this method has an insufficiently high fire resistance, which limits its use in a number of areas.
    technology. In addition, the process takes quite a long time.
    The aim of the invention is to accelerate the process and increase the fire resistance of the foam.
    This is achieved by using the cyclo-trimerization of an aromatic polyisocyanate in the presence of a polyol, a blowing agent and a mixture of N-D-methylcyclohexylamine and a salt of a saturated carboxylic acid, as a salt of a saturated carboxylic acid in the method of producing a foam with an isocyanuate structure by cyclo-trimerization of a saturated carboxylic acid for the equivalent of polysocyanate 20-80% solution of tetraalkylammonium salt of saturated carboxylic acid in ethylene glycol, and alkyl and carbonic acid contain 1-8 carbon atoms.
    This salt is obtained by reacting the corresponding diluted carboxylic acid with the corresponding quaternary ammonium hydroxide.
    The polyols used to make polycyanurate foams can be any. Potential 37 liols can be added separately during the trimerization of the polyisocyanate, or a preliminary reaction can be carried out with the polyisocyanate to produce a prepolymer with terminal isocyanate groups, which is then measured. The polyols are preferably used in an amount of from 0.01 equivalents to 0.5 equivalents per equivalent of isocyanate. The polyisocyanates used to make the polyisocyanuate foams can be any commonly used for this purpose. A particularly preferred polymethylene polyphenyl polyisocyan atom is one in which 30-85 wt.% Of methylene bis-phenyl isocyanate is contained. Blowing agents and other adjuvants, such as dispersing agents, stabilizers, surfactants, flame retardants, etc., can be used. A particularly preferred class of flame suppressant additives are tris (2-chloro-1-phosphate, tris). - (2-chloropropsh) -phosphate, tris- (2,3-; schromopropyl) -phosphate, tris- (1,3-dichloroisopropyl) -phosphate ug. n The proposed composition is applied by spraying in the form of heat- and fire-resistant polyisocent foams. Standard equipment can be used. It includes various types of sprayers. Foams show good adhesion to different substrates, including masonite, builder cardboard, gypsum plates, asbestos plates (transit), wood, plywood, sheet metal, all and paper products such as kraft paper and heavy cardboard. Heat: - and fire resistant foams, have good physical properties. When spraying, the foam cures quickly. They are sprayed at 4.4 ° C, including the temperature of the substrate. Foams have performance characteristics similar to those of simple polyurethane. This allows foam to be deposited in a thin layer. Example 1. Foam I is prepared from components A and B at 63-66 ° C. Spraying is carried out on cardboard and on stainless steel with excellent adhesion in both cases. Component A is polymethylene polyphenyl isocyanate, containing about 40% by weight of methylene-bass-phenyl-cyanate, the remainder of the mixture is polymethylene polyphenyl isocyanate with functionality higher than 2.0 and having an isocyanate equivalent weight of about 140. Component B is an insignificant amount of polyol, surfactant, blowing agent and catalytic composition. Formulation and properties are given in table. 1. Trimer content in foam I - 8.5%. The calculated trimer content is 8.12%. Example 2. Foam II is prepared analogously to example 1. Foam is sprayed onto a transit and good adhesion properties are obtained, netiy III is prepared analogously, but exclude treg-amine. The foam is sprayed onto the transit. The characteristics of the foam are identical to the foam I. However; Compared with the characteristics of foam II, foam III gives very poor adhesion to the transit and falls off the sheet. The composition and properties of pen II and are presented in table. 2. Example 3. Foams IV and V are prepared analogously to example I. However, foam IV is sprayed at ambient temperature (21 ° C), while foam V is sprayed at 4.4 ° C. Substrates in each case have the same temperature Foam IV and V spraying tests were carried out on cardboard and steel sheet. Excellent adhesion of foam was obtained for both foams. In tab. Figure 3 shows the formulation and physical properties of foams IV and V. Example 4. Samples of pen VI-XIV are prepared analogously to example 3, except when using ammonium salts. At room temperature, components A and B are thoroughly mixed for 3 and quickly poured onto cardboard foxes at 21 ° C and 4 ° C and onto steel sheets at 4 ° C. Foams are tested for adhesion after 2 minutes after the windows: the tubs are lifted off the steel or cardboard. In all cases, cardboard or steel, at 21 ° C or 4 ° C, the foam burst before it was separated from the substrate, which indicates excellent adhesion. Foams VI, VI and VIII are prepared with ammonium salt. Foams IX, X and XI. prepared with tetramethylammonium octoate and foam. XII, XIII and XIV with acetone tetraztilammonium. All foams have similar physical properties, regardless of the substrate temperature. A sample of foam VIII, but N, N-dimethylcyclohexylamine and poured onto a steel sheet at 4 ° C, gives poor adhesion to steel. Ethylene glycol is used to dissolve the ammonium salt in all cases. In tab. 4 The recipe and physical properties of VI-XIV foams. In tab. 5 shows the formulation and physical properties of the foams on the proposed and known method. In this way, a foam is obtained with greater fire resistance and in a shorter time than according to the known method. Indicator, unit of measure Component A Component B: polyester complex | LA-700 tris- (l-chloropropyl) -phosphate catalyst 1 M.Y.-dimethylcyclohexylamine DS-193 Freon PB Volume A / B ratio Weight weight A / B Period, s: 1 initiation 2 gel formation of the final foam lift without stick foam hardening Density, g / cm Test (ASTM D-1940) (cell closure), unit K-factor, unit. Flame spread, h / cm Crumb (ASTM D-4 wt.% Wet aging at W 0% relative humidity and 70 ° C D volume 14 days Dry aging at,% D about Compressive strength, kg / cm II lifting foam 1 lifting foam Oxygen index% Smoke density,% Spread rate (ASTM flame. Notes to Table 1 J. Polyester obtained 1 mol of chlorendic diethylene glycol anhydride and 2.5 moles approx. 2. Polyester for rigid hydroxyl penes 700. 3. Solution containing 60 the weight of tetramethylammonium sanoate and glycol is 20. 4. Silicone surface coating 5. Trichlorofluoromethane. 6. Percentage of oxygen required (more than to maintain the burning of the sample (ASTM D-2863) .. 7. Percentage of light absorption (ASTM D2843-7Q). Tabl i c 2 Note to Table 2 1. Solution containing 65% by weight of tetramethylammonium 2-ethylhexaoate and 35% by weight of ethylene glyol Table 3 Component B: polyester I tris- (/ 3-chloropropyl) phosphate catalyst 1 N, N-dimethylcyclohexylamine Freon 11-B component temperature, C ambient temperature, A / B lot ratio. kg / m good aging at 100% moisture content, and 70 C volume Cardboard Cardboard Carto Substrate 333 Mixing, from 555 Injection, from 151515 Thickening, with Lift, from 25 25
    Continued table. 3 arton Cardboard Steel Cardboard Cardboard Steel 333333 555777 1515151520 20 Adhesion to the substrate Density, kg / m 24.7 25.2 25.3 28.0 28.1 28.1 Oxygen index,% Distribution rate 100 100 100 smoke, unit Durability, in compression kg / cm 1,125 1,336 1,477
    Component A
    Note: 1.52% by weight of tetramethylammonium 2-eth1hexanoate and 48% by weight of ethylene glycol.
    2.50% by weight of 2-E1YALhexanoate and 50% by weight of ethylene glycol
    3. In | spelling during burning.
    ten
    718014
    Continued table. 4 in
    Table 5
    0.957 134 0.957
    134 of all samples is very good 26.5 25.9 26.3 23.723.7 23.5 29.6 23.6 29.1 28.027 28 200 100 100 100100 1.758 1.758 2.039 1.125 0.914 0.984
    11718014 12
    权利要求:
    Claims (1)
    [1]
    The claims of the invention are 0.0055-0.02 11 vivants per equivalent
    Spooob tioAji einut peybShvS c) fata al1-111mmmonium salt of a carbonated 1011c saturated carbonate with trimeric aromatic acid in ethylene glycol, and alkyl
    Schuitsch 1p6) 1SheOisig1Na | in 7L1r1 (carboxylic acid is present in the range of 1–8 atoms, sticking aretrra and mixtures of N, N-di-carbon.
    Me fftutufbi eiccfnnaMtma and associated with it.
    Carbovoy KIOSH1G 1, b tl and h ay ut and, with that, Sources of information,
    what, with UejiKio ush | yen process and hdJabtiiteiuiH taken into account during the examination
    fire resistance SbgO11 | ddu) y, 8 as Yu 1. Patent of Great Britain No. 1223415, SALT of carboxylic acid is used. C 3 R, pub. 1971 (prototype).
    polyisocyanate 20-80% solution of tetra
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    同族专利:
    公开号 | 公开日
    ZA753844B|1976-05-26|
    AU8220975A|1976-12-23|
    US3989651A|1976-11-02|
    USB486828I5|1976-03-02|
    CA1037649A|1978-08-29|
    ES439265A1|1977-03-01|
    GB1489819A|1977-10-26|
    DE2527241B2|1978-04-27|
    JPS5216760B2|1977-05-11|
    IT1040706B|1979-12-20|
    JPS5131795A|1976-03-18|
    BE831159A|1976-01-09|
    DD120035A5|1976-05-20|
    DE2527241A1|1976-02-05|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2779689A|1955-07-19|1957-01-29|Pittsburgh Plate Glass Co|Forming foamed polyurethane resins|
    BE587687A|1959-01-17|
    GB1155768A|1966-02-18|1969-06-18|Nisshin Boseki Kabushiki Kaish|Flame Resistant, Rigid Foams and a method for the preparation of the same|
    GB1200542A|1967-01-19|1970-07-29|Takeda Chemical Industries Ltd|A method for producing isocyanate trimers|
    US3745133A|1968-02-05|1973-07-10|Upjohn Co|Cellular isocyanurate containing polymers|
    US3849349A|1971-05-12|1974-11-19|K Frisch|Polyisocyanurate foam and process for producing the same|
    US3816339A|1972-02-22|1974-06-11|Abbott Lab|Urethane catalyst|
    US3892687A|1973-07-09|1975-07-01|Air Prod & Chem|Quaternary hydroxyalkyl tertiary amine bases as poluyrethane catalysts|JPS53140730U|1977-04-11|1978-11-07|
    US4136240A|1978-03-13|1979-01-23|Texaco Development Corporation|Metallic quaternary ammonium carboxylates as polyisocyanurate catalysts|
    US4198316A|1978-04-18|1980-04-15|Gaf Corporation|Foaming composition for textile finishing and coatings|
    JPS54167548U|1978-05-17|1979-11-26|
    DE2834119C2|1978-08-03|1981-01-15|Bayer Ag, 5090 Leverkusen|Process for the production of organopolysiloxane molding compounds which result in fine-pored, rubber-elastic molded foam bodies|
    US4503226A|1984-04-30|1985-03-05|Olin Corporation|Process for trimerizing organic polyisocyanates|
    CA1288546C|1986-11-14|1991-09-03|Ragui Ghali|Foam, composition and method of production|
    GB2217631A|1988-03-31|1989-11-01|Westinghouse Electric Corp|Method for attenuating gas diffusion through a structure|
    US4981880A|1988-09-23|1991-01-01|The Dow Chemical Company|Process for making low density flexible polyisocyanurate-polyurethane foams|
    JPH0699533B2|1988-11-24|1994-12-07|アキレス株式会社|Method for producing urethane-modified polyisocyanurate foam|
    DE10033099A1|2000-07-07|2002-01-17|Degussa|Process for the preparation of low-odor and storage-stable monomer-containing polyisocyanurates from isophorone diisocyanate|
    KR100895663B1|2001-08-31|2009-05-07|다이하치 카가쿠 고교 가부시키가이샤|Composition for production of flame-retardant flexible polyurethane foams|
    US7855240B2|2003-08-20|2010-12-21|Basf Corporation|Formulated resin component for use in spray-in-place foam system to produce a low density polyurethane foam|
    US7402277B2|2006-02-07|2008-07-22|Exxonmobil Research And Engineering Company|Method of forming metal foams by cold spray technique|
    US8580864B2|2006-05-04|2013-11-12|Air Products And Chemicals, Inc.|Trimer catalysts with improved processability and surface cure|
    US8530534B2|2006-05-04|2013-09-10|Air Products And Chemicals, Inc.|Trimerization catalysts from sterically hindered salts|
    US8552077B2|2006-05-04|2013-10-08|Air Products And Chemicals, Inc.|Trimer catalyst additives for improving foam processability|
    US8445555B2|2006-07-13|2013-05-21|Air Products And Chemicals, Inc.|Stabilized carbanions as trimerization catalysts|
    US20080312351A1|2007-06-13|2008-12-18|Air Products And Chemicals, Inc.|Tetraalkylammonium Carboxylate Salts as Trimerization Catalysts for Spray Foam Applications|
    WO2021043853A1|2019-09-04|2021-03-11|Evonik Operations Gmbh|Phase transfer active trimerization catalyst salts|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/486,828|US3989651A|1974-07-09|1974-07-09|Catalyst for sprayable polyisocyanurate foam composition|
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