Preparation method of hydrotalcite and polyimide composite foam material

Abstract

The invention provides a preparation method of a hydrotalcite and polyimide composite foam material. Aromatic dianhydride is heated and dissolved in a polar solvent to react with fatty alcohol to obtain an aromatic dianhydride derivative diacid diester liquor; the diacid diester liquor is compounded with a foam stabilizer to form combined liquor; hydrotalcite is filled in and sufficiently stirred to form a uniform milk white material; polyisocyanates are added and quickly stirred uniformly to form mixed liquor, and the mixed liquor is quickly poured into a mould for freely foaming to obtain a foam plastic intermediate; the foam intermediate is prepared into the hydrotalcite and polyimide composite foam material by electric-heating and curing. The foam plastic prepared by the preparation method has a semi-closed structure, is uniform in foam holes and is soft in texture; the hydrotalcite achieves smoke inhibition effect while improving material flame resistance. The preparation method disclosed by the invention is simple in process, low in cost and easy to industrially produce. Besides, the product is excellent in flame resistance, and can satisfy fireproof safety requirements in a using process of a thermal-insulation heat insulating material.

Description

technical field

[0001] The invention relates to a preparation method of a high-temperature resistant flame-retardant composite foam material, in particular to a preparation method of a hydrotalcite / polyimide composite foam material. Background technique

[0002] Polyimide foam is a kind of lightweight porous material with high-performance polymer material-polyimide as the matrix resin. Due to its high thermal stability, thermal insulation, sound absorption, and flame retardant Excellent performance, low smoke generation during combustion, etc., have been widely concerned and applied in cutting-edge technical fields such as aerospace, ships, and high-speed trains. Although the polyimide foam produced by the two-step method has excellent overall performance, the price of the product is expensive due to special process equipment, long preparation process lines, and complicated production processes, so it is limited to relevant civil applications with lower performance requireme...

Examples

preparation example Construction

[0033] The preparation method of the hydrotalcite / polyimide composite foam material is characterized in that: the hydrotalcite includes: binary and ternary components composed of magnesium, aluminum, nickel, calcium, copper and rare earth metal elements. Hydrotalcite.

[0034] The aromatic dianhydrides include: pyromellitic dianhydride (PMDA), 3,3′,4,4′-benzophenone tetraacid dianhydride (BTDA), 3,3′,4,4′- Biphenyl tetra-acid dianhydride (BPDA), 3,3′,4,4′-diphenyl ether tetra-acid dianhydride (ODPA), 3,3′,4,4′-biphenyl sulfone tetracarboxylic acid di anhydride (DSDA).

[0035] The polar solvent includes: N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and dimethylsulfoxide.

[0036] Described fatty alcohol comprises: methyl alcohol, ethanol.

[0037] The foam stabilizers include: non-hydrolyzable water-soluble polyether siloxane (AK8805, DC193, L580); surfactants include: non-ionic fluorocarbon surfactants ( FS-300, FSO-100), polyethylene oxide nonion...

Embodiment 1

[0042] In a 500ml three-necked flask, add 160 grams of N,N-dimethylformamide and 100 grams of 3,3′,4,4′-benzophenone tetra-acid dianhydride (BTDA) into the magnetic sub, and connect to reflux condensation Put cooling water into the tube, fully stir under the action of an electromagnetic stirrer and slowly raise the temperature to 110°C until the 3,3′,4,4′-benzophenone tetraacid dianhydride (BTDA) is completely dissolved and the solution is in a clear state Stop heating, and when the temperature drops to about 50°C, drop 18 grams of methanol into the turbid liquid with a constant pressure dropping funnel, and the dropping rate is controlled at 1-5 ml per minute, so that 3, 3', 4, 4' - Benzophenone tetra-acid dianhydride (BTDA) begins to undergo esterification reaction. After the esterification reaction is complete and the solution is clear and transparent again, the electromagnetic stirrer stops stirring, and the above solution is left to stand at room temperature to obtain a ne...

Embodiment 2

[0051] Take by weighing 20 grams of the diacid diester solution described in Example 1, add 3 grams of foam stabilizer, 3 grams of polyoxyethylene surfactant, 0.3 gram of fluorocarbon surfactant, 3 grams of composite catalyst, 5 grams of deionized water , After fully stirring, a clear and transparent foam combination solution is formed. Add 15 grams of nickel-aluminum hydrotalcite powder into the clear foam combination solution, and disperse under the action of ultrasonic waves to obtain a white emulsion.

[0052] Stir the white emulsion and 30 grams of polyphenyl polymethylene polyisocyanate with an electric stirring paddle quickly and evenly. When the mixture starts to foam and rises, it is quickly poured into the mold to foam freely. The foam intermediate is at room temperature. After standing still for 5 minutes, transfer to an electric blast drying oven heated to 180° C. for curing for 120 minutes to obtain a polyimide foam.

[0053] The relevant properties and propertie...

technical field

[0001] The invention relates to a preparation method of a high-temperature resistant flame-retardant composite foam material, in particular to a preparation method of a hydrotalcite / polyimide composite foam material. Background technique

[0002] Polyimide foam is a kind of lightweight porous material with high-performance polymer material-polyimide as the matrix resin. Due to its high thermal stability, thermal insulation, sound absorption, and flame retardant Excellent performance, low smoke generation during combustion, etc., have been widely concerned and applied in cutting-edge technical fields such as aerospace, ships, and high-speed trains. Although the polyimide foam produced by the two-step method has excellent overall performance, the price of the product is expensive due to special process equipment, long preparation process lines, and complicated production processes, so it is limited to relevant civil applications with lower performance requireme...

Examples

preparation example Construction

[0033] The preparation method of the hydrotalcite / polyimide composite foam material is characterized in that: the hydrotalcite includes: binary and ternary components composed of magnesium, aluminum, nickel, calcium, copper and rare earth metal elements. Hydrotalcite.

[0034] The aromatic dianhydrides include: pyromellitic dianhydride (PMDA), 3,3′,4,4′-benzophenone tetraacid dianhydride (BTDA), 3,3′,4,4′- Biphenyl tetra-acid dianhydride (BPDA), 3,3′,4,4′-diphenyl ether tetra-acid dianhydride (ODPA), 3,3′,4,4′-biphenyl sulfone tetracarboxylic acid di anhydride (DSDA).

[0035] The polar solvent includes: N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and dimethylsulfoxide.

[0036] Described fatty alcohol comprises: methyl alcohol, ethanol.

[0037] The foam stabilizers include: non-hydrolyzable water-soluble polyether siloxane (AK8805, DC193, L580); surfactants include: non-ionic fluorocarbon surfactants ( FS-300, FSO-100), polyethylene oxide nonion...

Embodiment 1

[0042] In a 500ml three-necked flask, add 160 grams of N,N-dimethylformamide and 100 grams of 3,3′,4,4′-benzophenone tetra-acid dianhydride (BTDA) into the magnetic sub, and connect to reflux condensation Put cooling water into the tube, fully stir under the action of an electromagnetic stirrer and slowly raise the temperature to 110°C until the 3,3′,4,4′-benzophenone tetraacid dianhydride (BTDA) is completely dissolved and the solution is in a clear state Stop heating, and when the temperature drops to about 50°C, drop 18 grams of methanol into the turbid liquid with a constant pressure dropping funnel, and the dropping rate is controlled at 1-5 ml per minute, so that 3, 3', 4, 4' - Benzophenone tetra-acid dianhydride (BTDA) begins to undergo esterification reaction. After the esterification reaction is complete and the solution is clear and transparent again, the electromagnetic stirrer stops stirring, and the above solution is left to stand at room temperature to obtain a ne...

Embodiment 2

[0051] Take by weighing 20 grams of the diacid diester solution described in Example 1, add 3 grams of foam stabilizer, 3 grams of polyoxyethylene surfactant, 0.3 gram of fluorocarbon surfactant, 3 grams of composite catalyst, 5 grams of deionized water , After fully stirring, a clear and transparent foam combination solution is formed. Add 15 grams of nickel-aluminum hydrotalcite powder into the clear foam combination solution, and disperse under the action of ultrasonic waves to obtain a white emulsion.

[0052] Stir the white emulsion and 30 grams of polyphenyl polymethylene polyisocyanate with an electric stirring paddle quickly and evenly. When the mixture starts to foam and rises, it is quickly poured into the mold to foam freely. The foam intermediate is at room temperature. After standing still for 5 minutes, transfer to an electric blast drying oven heated to 180° C. for curing for 120 minutes to obtain a polyimide foam.

[0053] The relevant properties and propertie...