Preparation method of hydrotalcite and polyimide composite foam material

A polyimide and composite foam technology, which is applied in the field of preparation of hydrotalcite/polyimide composite foam materials, can solve the slow reaction speed of aromatic diacid diester, reduce the flame retardancy of materials, low reaction degree, etc. problem, to achieve the effect of uniform cells, improved flame retardancy, and simple preparation process

Inactive Publication Date: 2014-07-02
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is simple, the process is still relatively complicated. At the same time, due to the slow reaction speed and low degree of reaction between

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

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

[0034] The aromatic dianhydride includes: pyromellitic dianhydride (PMDA), 3,3′,4,4′-benzophenonetetracarboxylic dianhydride (BTDA), 3,3′,4,4′- Biphenyltetracarboxylic dianhydride (BPDA), 3,3′,4,4′-diphenyl ether tetracarboxylic dianhydride (ODPA), 3,3′,4,4′-biphenylsulfone tetracarboxylic acid two Anhydride (DSDA).

[0035] The polar solvents include: N-methylpyrrolidone, N,N-dimethylformamide, N,N-dimethylacetamide, and dimethylsulfoxide.

[0036] The fatty alcohols include: methanol and ethanol.

[0037] The foam stabilizer includes: non-hydrolyzable water-soluble polyether siloxane (AK8805, DC193, L580); surfactant includes: non-ionic fluorocarbon surfactant ( FS-300, FSO-100), polyethylene oxide non-ionic surfacta...

Example Embodiment

[0041] Implementation example 1:

[0042] In a 500ml three-necked flask, add 160 grams of N,N-dimethylformamide and 100 grams of 3,3′,4,4′-benzophenonetetracarboxylic dianhydride (BTDA), add magnets, and then reflux for condensation Fill the tube with cooling water, stir fully under the action of an electromagnetic stirrer and slowly raise the temperature to 110°C. When the 3,3′,4,4′-benzophenonetetracarboxylic dianhydride (BTDA) is completely dissolved and the solution is clear Stop heating, and when the temperature drops to about 50℃, 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 to make 3,3',4,4' -Benzophenone tetraacid dianhydride (BTDA) starts to undergo esterification reaction. After the esterification reaction is complete and the solution becomes clear and transparent again, the electromagnetic stirrer stops stirring, and the above solution is allowed to stand still to roo...

Example Embodiment

[0050] Implementation example 2:

[0051] Weigh 20 grams of the diacid diester solution described in Example 1, add 3 grams of foam stabilizer, 3 grams of polyethylene oxide surfactant, 0.3 grams of fluorocarbon surfactant, 3 grams of compound catalyst, and 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 to the clear foam combination solution, and disperse under the action of ultrasound to obtain a white emulsion.

[0052] Quickly stir the white emulsion and 30 grams of polyphenyl polymethylene polyisocyanate with an electric stirring blade. When the mixture starts to foam and rise, quickly pour it into the mold and foam freely. The foam intermediate is at room temperature. After standing for 5 minutes, it was transferred to an electric heating blast drying oven preheated to 180° C. and cured for 120 minutes to obtain polyimide foam.

[0053] Related properties and pr...

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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...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08G73/10C08K3/26C08J9/00
CPCC08K3/26C08G73/1035C08K2003/265C08L2201/02C08L2201/08C08L2203/14
Inventor 刘连河孙高辉韩世辉王君魏浩王洪良
Owner HARBIN ENG UNIV
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