CN103012777A - High temperature resistant semi-aromatic polyamide, preparation method and applications thereof - Google Patents
High temperature resistant semi-aromatic polyamide, preparation method and applications thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of polymer materials, and discloses a high temperature resistant semi-aromatic polyamide, a preparation method and applications thereof. The high temperature resistant semi-aromatic polyamide is prepared from the following components, by weight, 20-60 wt% of a nylon salt formed from m-phthalic acid and aliphatic diamine, 30-70 wt% of a nylon salt formed from p-phthalic acid and aliphatic diamine, and 1-15 wt% of a multi-functional group active monomer substance. The preparation method comprises the following steps: adding 20-60 wt% of a nylon salt formed from m-phthalic acid and aliphatic diamine, 30-70 wt% of a nylon salt formed from p-phthalic acid and aliphatic diamine, 1-15 wt% of a multi-functional group active monomer substance, and water to a polymerization kettle, wherein a use amount of the water is 20-200 wt% of the total weight of the three raw materials; vacuumizing and introducing nitrogen; and carrying out heating condensation polymerization to prepare the semi-aromatic polyamide. The present invention further discloses a method for adopting the high temperature resistant semi-aromatic polyamide as an adhesive to adhere a metal. The product of the present invention has good curing stability.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of high temperature resistant semiaromatic polyamide composition, preparation method and application thereof.
Background technology
Develop rapidly along with high-tech, people are more and more higher to the requirement of material, and especially to the application requiring expanding day of non-metallic material, therefore, the restriction that is connected to become between structural part or the non-structural part much has the bottleneck that the excellent properties material is used.Tackiness agent can partly replace traditional welding as the important material that can be used for the material connection, and riveted joint or bolt connect, even can be used for can't or riveting the position that connects with welding at all.
In the continuous progress and development of tackiness agent, working temperature to the thermotolerance tackiness agent requires also more and more higher, often being used to has epoxyn (such as Chinese patent CN101139510 as the product of high-temperature resistance adhesive, CN101157835, CN101186796), synvaren is (such as Chinese patent: CN 101921565A), in recent years because electrical/electronic, the development of aerospace industry, temperature resistant grade to tackiness agent requires also more and more higher, but the temperature resistant grade of these existing tackiness agent can't meet the demands, and fragrant heterocyclic polymer uses as high-temperature resistance adhesive and receives increasing concern.For example polyimide virtue heterocyclic polymer by constantly research, improve, and be applied to the aspect (such as Chinese patent: CN 1445324A and CN 101580687A) of high-temperature resistance adhesive.But polyimides adhesive cost in commercial process is higher, and many places are in conceptual phase.
The semiaromatic polyamide composition that the present invention is intended to be in recent years ascent stage and to have a good prospect in the high temperature resistant nylon industry is incorporated into the high-temperature resistance adhesive application facet.Semi-aromatic polyamide is by aliphatie diamine or diacid and with diacid or the diamines of aromatic nucleus, gets through polycondensation.Because in Wholly aromatic polyamide molecular backbone chain section, having introduced aliphatic chain, increased the kindliness of chain, cost performance is high, is that the high heat resistance resin between general engineering plastic and thermostability engineering plastic PEEK has a wide range of applications at automobile and electric industrial circle.The production technique of semiaromatic polyamide composition is simple, and has environment friendly.The present invention introduces the polyfunctional group structure in semiaromatic polyamide composition, make it form the interpenetrating net polymer structure, further improves heatproof rank, high-temperature stability and the solvent resistance of semiaromatic polyamide composition.
Summary of the invention
For the problem of prior art, the object of the invention provides a kind of high temperature resistant semiaromatic polyamide composition, and this semiaromatic polyamide composition can be used as tackiness agent, enlarges its Application Areas in the prior art.
Another object of the present invention provides a kind of preparation method of above-mentioned high temperature resistant semiaromatic polyamide composition.
The 3rd purpose of the present invention provides a kind of with the method for above-mentioned high temperature resistant semiaromatic polyamide composition as the adhesive bonds metal.
Technical scheme of the present invention is as follows:
The invention provides a kind of high temperature resistant semiaromatic polyamide composition, this high temperature resistant semiaromatic polyamide composition is made by the component that comprises following weight percentage:
The nylon salt that the m-phthalic acid of 20～60wt% and aliphatie diamine form;
The nylon salt that the terephthalic acid of 30～70wt% and aliphatie diamine form;
The polyfunctional group reactive monomer material of 1～15wt%.
The structure of described aliphatie diamine is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in 12 carbon amine, decamethylene diamine, nonamethylene diamine or the octamethylenediamine.
The nylon salt structure that described m-phthalic acid and aliphatie diamine form is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in m-phthalic acid 12 carbon amine salt (12I salt), m-phthalic acid decamethylene diamine salt (10I salt), m-phthalic acid nonamethylene diamine salt (9I salt) or the m-phthalic acid octamethylenediamine salt (8I salt).
The nylon salt structure that described terephthalic acid and fat family diamines form is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in terephthalic acid 12 carbon amine salt (12T salt), terephthalic acid decamethylene diamine salt (10T salt), terephthalic acid nonamethylene diamine salt (9T salt) or the terephthalic acid octamethylenediamine salt (8T salt).
Described polyfunctional group reactive monomer material is selected from one or more the material in polyamine or the polyvalent alcohol; Wherein: polyamine further is selected from one or more the material in equal benzene tetramine or the trimeric cyanamide, is preferably trimeric cyanamide; Polyvalent alcohol further is selected from one or more the material in tetramethylolmethane, glycerol or the trimethylolethane, is preferably trimethylolethane.
The present invention also provides a kind of preparation method of above-mentioned high temperature resistant semiaromatic polyamide composition, the method may further comprise the steps: be the nylon salt that the m-phthalic acid of 20～60wt% and aliphatie diamine form with weight percentage, weight percentage is the terephthalic acid of 30～70wt% and the nylon salt that aliphatie diamine forms, weight percentage is that polyfunctional group reactive monomer material and the water of 1～15wt% joins in the polymeric kettle together, the consumption of water is 20～200wt% of above-mentioned three kinds of raw material gross weights, vacuumize, pass into nitrogen, prepare semiaromatic polyamide composition after the intensification polycondensation.
The consumption of described water is 40～150wt% of three kinds of raw material gross weights, is preferably 50～130wt%.
The described pressure that passes into nitrogen is 1.8～3.2Mpa.
The temperature of reaction of described intensification polycondensation is 200～260 ℃, and the reaction times is 2～5 hours.
Described vacuumizing is in order to remove the air in the still, to prevent that the existence because of oxygen in the air from affecting the preparation of semiaromatic polyamide composition.
It is a kind of with the method for above-mentioned high temperature resistant semiaromatic polyamide composition as the adhesive bonds metal that the present invention also provides, the method may further comprise the steps: the semiaromatic polyamide composition for preparing is dissolved in obtains semiaromatic polyamide composition solution in the organic solvent, then semiaromatic polyamide composition solution is coated on bonded metallic surface, compress, 250～340 ℃ of lower curing 1～3 hour, obtain firmly cohesive body.
Described organic solvent is selected from N, and the material of one or more in N '-dimethyl formamide, N,N-DIMETHYLACETAMIDE or the METHYLPYRROLIDONE is preferably N, N '-dimethyl formamide.
The mass concentration of described semiaromatic polyamide composition solution is 30-95wt%, is preferably 50-90wt%, more preferably 65-80wt%.
It is clean that the polished finish polishing is carried out in described metallic surface, gets rid of impurity.
The present invention compares with prior art, has the following advantages and beneficial effect:
1, the present invention is applied to the tackiness agent aspect with semiaromatic polyamide composition, enlarges the application of semiaromatic polyamide composition.
2, prepare first the semiaromatic polyamide composition primary polymer among the present invention, the preparation method of primary polymer is simple, and is pollution-free, and the preparation the semiaromatic polyamide composition primary polymer be pulverulence, good stability is conducive to next step use.
3, the present invention can improve the kindliness of semiaromatic polyamide composition molecular chain with following two kinds of structure copolymerization together, thereby is conducive to improve toughness and the degree of adhesion of final semiaromatic polyamide composition tackiness agent.
4, the present invention adds polyfunctional group reactive monomer (following structural formula) in semiaromatic polyamide composition, can make the semiaromatic polyamide composition tackiness agent form interpenetrating polymer networks (IPN) structure, thereby make the heat resisting temperature of semiaromatic polyamide composition tackiness agent bring up to 350-450 ℃ from 270～310 ℃; And the formation of interpenetrating polymer networks structure makes the semiaromatic polyamide composition tackiness agent possess more excellent solvent resistance, stability and better mechanical property.
5, semiaromatic polyamide composition of the present invention can be used for the welding of high temperature resistant position circuit in the bonding and circuit card of metal, and its room temperature stripping strength can reach 60KN/m; Shearing resistance is 200 ℃, 25.33MPa, 250 ℃, 18.45MPa, 280 ℃, 10.25MPa, 300 ℃, 5.67MPa, 350 ℃, 2.32MPa.
6, semiaromatic polyamide composition of the present invention is stablized, and is easy to use, and stronger for the semiaromatic polyamide composition tackiness agent stability after solidifying, its temperature resistant grade is high, and solvent resistance is excellent.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
The preparation process of semiaromatic polyamide composition can be divided into for two steps among the present invention, at first be that nylon salt is prepared into the semi-aromatic nylon primary polymer under given conditions, then in application process, primary polymer is dissolved in the organic solvent, after be cured through heating and obtain semiaromatic polyamide composition adhesive solidification thing.
The nylon salt that the nylon salt that the m-phthalic acid that present embodiment is used and aliphatie diamine form and terephthalic acid and aliphatie diamine form is to adopt page 1 to the disclosed method of page 2 in illustrating among the Chinese patent CN 1887841A to prepare.
The concrete preparation process of nylon salt is as follows:
M-phthalic acid or terephthalic acid are added in the dissolution kettle, add 2-5 doubly with respect to the water of sour weight again, be heated to while stirring 60-105 ℃, it is stand-by to obtain acid solution, aliphatic diamine is dissolved in the water of 1-2 times of weight simultaneously, being heated to 60-100 ℃, to obtain amine aqueous solution stand-by.Acid and amine aqueous solution are entered the hybrid reactor internal reaction according to equimolar ratio with the metering infusion, and temperature of reaction is controlled at 60-95 ℃, and reaction end is PH 7.0-7.2.Again salts solution is injected crystallizer, obtain the nylon salt of m-phthalic acid and aliphatie diamine formation or the nylon salt of terephthalic acid and aliphatie diamine formation through crystallisation by cooling.
The semi-aromatic nylon primary polymer that requires among the present invention to utilize the nylon salt preparation is under 30 ℃, and intrinsic viscosity is 0.1-0.2dl/g in the vitriol oil.Molecular chain keeps linear structure in the prepolymer under this intrinsic viscosity, and the molecular chain end group has good reactive behavior, and further polymerization easily forms interpenetrating polymer networks (IPN) structure in next step solidification process.
The intrinsic viscosity measuring method is as follows among the present invention: the semiaromatic polyamide composition prepolymer is dissolved in the vitriol oil, obtains concentration and be 0.05,0.1,0.2 or the solution of 0.4dl/g, get 30 ℃ of lower logarithmic viscosity number η that measure each sample solution
Rlh,
η
rlh＝[In(t/t
0)]/C
T wherein
0The flushing time (s) of expression solvent, t represents the flushing time (s) of sample solution, C represents the concentration of sample in the sample solution.With η
RlhData Extrapolation be 0 scope to concentration, to obtain the intrinsic viscosity of sample
The stripping strength of semiaromatic polyamide composition tackiness agent is tested according to the GB-T2791-1995 method of inspection among the present invention.
Embodiment 1
Composition of raw materials:
The m-phthalic acid decamethylene diamine salt (10I salt) of 40wt%
The terephthalic acid decamethylene diamine salt (10T salt) of 45wt%
The trimeric cyanamide of 15wt%
According to said ratio, taking by weighing each component raw material joins in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 50%), vacuumize, pass into nitrogen to still internal pressure and reach 2.0MPa, be warming up to 200 ℃, reacted 3 hours, and prepared the semiaromatic polyamide composition that intrinsic viscosity is 0.1dl/g.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 78wt%.With this adhesive bonds aluminium alloy, before the bonding aluminum alloy surface is carried out polished finish, bright clean with the emery paper polishing, get rid of impurity.Then semiaromatic polyamide composition adhesive solvent on coated on both sides compresses after the bonding of two sides, solidifies in 250 ℃ to obtain firmly aluminium alloy-aluminium alloy cohesive body in 3 hours.
Aluminium alloy-aluminium alloy adhesive property:
The room temperature stripping strength can reach 62KN/m;
Shearing resistance is 200 ℃, 21.53MPa, 250 ℃, 16.42MPa, 280 ℃, 9.64MPa, 300 ℃, 4.02MPa, 330 ℃, 2.12MPa.
Embodiment 2
Composition of raw materials:
The m-phthalic acid nonamethylene diamine salt (9I salt) of 20wt%
The terephthalic acid nonamethylene diamine salt (9T salt) of 70wt%
The equal benzene tetramine of 6wt%
The trimeric cyanamide of 4wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 100%).Vacuumize, pass into nitrogen to still internal pressure and reach 1.8MPa, be warming up to 200 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.12dl/g in 4 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 68wt%.With this adhesive bonds aluminium alloy, before the bonding aluminum alloy surface is carried out polished finish, bright clean with the emery paper polishing, get rid of impurity.Then semiaromatic polyamide composition adhesive solvent on coated on both sides is pressed in 280 ℃ of curing and obtained firmly aluminium alloy-aluminium alloy cohesive body in 2 hours after the bonding of two sides.
Aluminium alloy-aluminium alloy adhesive property:
The room temperature stripping strength can reach 57KN/m;
Shearing resistance is 200 ℃, 23.54MPa, 250 ℃, 17.65MPa, 280 ℃, 9.46MPa, 300 ℃, 5.21MPa, 330 ℃, 1.98MPa.
Embodiment 3
Composition of raw materials:
The m-phthalic acid octamethylenediamine salt (8I salt) of 40wt%
The terephthalic acid octamethylenediamine salt (8T salt) of 55wt%
The trimeric cyanamide of 2wt%
The equal benzene tetramine of 3wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 130%).Vacuumize, pass into nitrogen to still internal pressure and reach 2.5MPa, be warming up to 260 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.15dl/g in 2 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 80wt%.With this adhesive bonds aluminium alloy, before the bonding aluminum alloy surface is carried out polished finish, bright clean with the emery paper polishing, get rid of impurity.Then semiaromatic polyamide composition adhesive solvent on coated on both sides is pressed in 290 ℃ of curing and obtained firmly aluminium alloy-aluminium alloy cohesive body in 2 hours after the bonding of two sides.
Aluminium alloy-aluminium alloy adhesive property:
The room temperature stripping strength can reach 55KN/m;
Shearing resistance is 200 ℃, 24.01MPa, 250 ℃, 17.56MPa, 280 ℃, 9.97MPa, 300 ℃, 5.46MPa, 330 ℃, 2.10MPa.
Embodiment 4
Composition of raw materials:
The m-phthalic acid 12 carbon amine salt (12I salt) of 35wt%
The terephthalic acid 12 carbon amine salt (12T salt) of 64wt%
The trimeric cyanamide of 1wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 100%).Vacuumize, pass into nitrogen to still internal pressure and reach 2.2MPa, be warming up to 200 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.16dl/g in 5 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 75wt%.With this adhesive bonds aluminium alloy, before the bonding aluminum alloy surface is carried out polished finish, bright clean with the emery paper polishing, get rid of impurity.Then semiaromatic polyamide composition adhesive solvent on coated on both sides is pressed in 300 ℃ of curing and obtained firmly aluminium alloy-aluminium alloy cohesive body in 1.5 hours after the bonding of two sides.
Aluminium alloy-aluminium alloy adhesive property:
The room temperature stripping strength can reach 62KN/m;
Shearing resistance is 200 ℃, 25.33MPa, 250 ℃, 18.45MPa, 280 ℃, 10.25MPa, 300 ℃, 5.67MPa, 330 ℃, 2.32MPa.
Embodiment 5
Composition of raw materials:
The m-phthalic acid 12 carbon amine salt (12I salt) of 20wt%
The m-phthalic acid octamethylenediamine salt (8I salt) of 40wt%
The terephthalic acid 12 carbon amine salt (12T salt) of 18wt%
The terephthalic acid decamethylene diamine salt (10T salt) of 15wt%
The trimethylolethane of 7wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 80%).Vacuumize, pass into nitrogen to still internal pressure and reach 2.0MPa, be warming up to 200 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.18dl/g in 5 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 70wt%.With this adhesive bonds aluminium alloy, before the bonding aluminum alloy surface is carried out polished finish, bright clean with the emery paper polishing, get rid of impurity.Then semiaromatic polyamide composition adhesive solvent on coated on both sides is pressed in 320 ℃ of curing and obtained firmly aluminium alloy-aluminium alloy cohesive body in 1 hour after the bonding of two sides.
Aluminium alloy-aluminium alloy adhesive property:
The room temperature stripping strength can reach 58KN/m;
Shearing resistance is 200 ℃, 23.98MPa, 250 ℃, 17.45MPa, 280 ℃, 8.76MPa, 300 ℃, 4.32MPa, 330 ℃, 2.21MPa.
Embodiment 6
Composition of raw materials:
The m-phthalic acid nonamethylene diamine salt (9I salt) of 32wt%
The terephthalic acid octamethylenediamine salt (8T salt) of 30wt%
The terephthalic acid nonamethylene diamine salt (9T salt) of 30wt%
The trimethylolethane of 8wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 100%).Vacuumize, pass into nitrogen to still internal pressure and reach 2.3MPa, be warming up to 245 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.2dl/g in 3 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 65wt%.This tackiness agent is used in the welding of circuit card circuit.Get ganoid copper wire and be immersed in the tackiness agent, then the coating part tackiness agent is in the circuit card corresponding position, and the copper wire that will soak tackiness agent is pressed on circuit board surface, and solidifies 1.5 hours at 340 ℃.
Its room temperature stripping strength can reach 60KN/m;
Shearing resistance is 200 ℃, 21.05MPa, 250 ℃, 15.67MPa, 280 ℃, 7.56MPa, 300 ℃, 3.25MPa, 330 ℃, 1.75MPa.
Embodiment 7
Composition of raw materials:
The m-phthalic acid 12 carbon amine salt (12I salt) of 23wt%
The m-phthalic acid decamethylene diamine salt (10I salt) of 35wt%
The terephthalic acid decamethylene diamine salt (10T salt) of 30wt%
The equal benzene tetramine of 2wt%
The trimeric cyanamide of 10wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 120%).Vacuumize, pass into nitrogen to still internal pressure and reach 2.0MPa, be warming up to 220 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.17dl/g in 4 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 72wt%.This tackiness agent is used in the welding of circuit card circuit.Get ganoid aluminum steel and be immersed in the tackiness agent, then with the coating part tackiness agent in the circuit card corresponding position, the copper wire that will soak tackiness agent is pressed on circuit board surface, and solidifies 2 hours at 310 ℃.
Its room temperature stripping strength can reach 57KN/m;
Shearing resistance is 200 ℃, 21.67MPa, 250 ℃, 14.91MPa, 280 ℃, 7.31MPa, 300 ℃, 2.89MPa, 330 ℃, 2.01MPa.
Embodiment 8
Composition of raw materials:
The m-phthalic acid decamethylene diamine salt (10I salt) of 24wt%
The terephthalic acid 12 carbon amine salt (12T salt) of 70wt%
The equal benzene tetramine of 6wt%
According to said ratio, take by weighing each component raw material and join in the polymeric kettle that contains water (consumption of water be above-mentioned each component gross weight 130%).Vacuumize, pass into nitrogen to still internal pressure and reach 3.2MPa, be warming up to 260 ℃, react and obtained the semiaromatic polyamide composition that intrinsic viscosity is 0.19dl/g in 2 hours.
The above-mentioned semiaromatic polyamide composition for preparing is dissolved in N, in N '-dimethyl formamide, obtains the semiaromatic polyamide composition adhesive solvent, this strength of solution is 77wt%.This tackiness agent is used in the welding of circuit card circuit.Get ganoid aluminum steel and be immersed in the tackiness agent, then with the coating part tackiness agent in the circuit card corresponding position, the copper wire that will soak tackiness agent is pressed on circuit board surface, and solidifies 3 hours at 300 ℃.
Its room temperature stripping strength can reach 53KN/m;
Shearing resistance is 200 ℃, 19.24MPa, 250 ℃, 13.25MPa, 280 ℃, 6.98MPa, 300 ℃ of 2.56MPa, 330 ℃, 1.99MPa.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not breaking away from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. high temperature resistant semiaromatic polyamide composition, it is characterized in that: this high temperature resistant semiaromatic polyamide composition is made by the component that comprises following weight percentage:
The nylon salt that the m-phthalic acid of 20～60wt% and aliphatie diamine form;
The nylon salt that the terephthalic acid of 30～70wt% and aliphatie diamine form;
The polyfunctional group reactive monomer material of 1～15wt%.
2. high temperature resistant semiaromatic polyamide composition according to claim 1, it is characterized in that: the structure of described aliphatie diamine is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in 12 carbon amine, decamethylene diamine, nonamethylene diamine or the octamethylenediamine.
3. high temperature resistant semiaromatic polyamide composition according to claim 1 is characterized in that: the nylon salt structure that described m-phthalic acid and aliphatie diamine form is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in m-phthalic acid 12 carbon amine salt, m-phthalic acid decamethylene diamine salt, m-phthalic acid nonamethylene diamine salt or the m-phthalic acid octamethylenediamine salt;
The nylon salt structure that described terephthalic acid and fat family diamines form is shown below:
Wherein: 8≤m≤12;
Be preferably one or more the material in terephthalic acid 12 carbon amine salt, terephthalic acid decamethylene diamine salt, terephthalic acid nonamethylene diamine salt or the terephthalic acid octamethylenediamine salt.
4. high temperature resistant semiaromatic polyamide composition according to claim 1 is characterized in that: described polyfunctional group reactive monomer material is selected from one or more the material in polyamine or the polyvalent alcohol; Wherein: polyamine further is selected from one or more the material in equal benzene tetramine or the trimeric cyanamide, is preferably trimeric cyanamide; Polyvalent alcohol further is selected from one or more the material in tetramethylolmethane, glycerol or the trimethylolethane, is preferably trimethylolethane.
5. the preparation method of the arbitrary described high temperature resistant semiaromatic polyamide composition of claim 1 to 4, it is characterized in that: the method may further comprise the steps: be the nylon salt that the m-phthalic acid of 20～60wt% and aliphatie diamine form with weight percentage, weight percentage is the terephthalic acid of 30～70wt% and the nylon salt that aliphatie diamine forms, weight percentage is that polyfunctional group reactive monomer material and the water of 1～15wt% joins in the polymeric kettle together, the consumption of water is 20～200wt% of above-mentioned three kinds of raw material gross weights, vacuumize, pass into nitrogen, prepare semiaromatic polyamide composition after the intensification polycondensation.
6. the preparation method of high temperature resistant semiaromatic polyamide composition according to claim 5, it is characterized in that: the consumption of described water is 40～150wt% of three kinds of raw material gross weights, is preferably 50～130wt%; The described pressure that passes into nitrogen is 1.8～3.2Mpa; The temperature of reaction of described intensification polycondensation is 200～260 ℃, and the reaction times is 2～5 hours.
7. the arbitrary described high temperature resistant semiaromatic polyamide composition of claim 1 to 4 is as the method for adhesive bonds metal, it is characterized in that: the method may further comprise the steps: the semiaromatic polyamide composition for preparing is dissolved in obtains semiaromatic polyamide composition solution in the organic solvent, then semiaromatic polyamide composition solution is coated on bonded metallic surface, compress, 250～340 ℃ of lower curing 1～3 hour, obtain firmly cohesive body.
8. high temperature resistant semiaromatic polyamide composition according to claim 7 is as the method for adhesive bonds metal, it is characterized in that: described organic solvent is selected from N, the material of one or more in N '-dimethyl formamide, N,N-DIMETHYLACETAMIDE or the METHYLPYRROLIDONE, be preferably N, N '-dimethyl formamide.
9. high temperature resistant semiaromatic polyamide composition according to claim 7 is as the method for adhesive bonds metal, and it is characterized in that: the mass concentration of described semiaromatic polyamide composition solution is 30-95wt%, is preferably 50-90wt%, more preferably 65-80wt%.
10. high temperature resistant semiaromatic polyamide composition according to claim 7 is as the method for adhesive bonds metal, and it is characterized in that: polished finish is carried out in described metallic surface.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497569A (en) * | 2014-12-17 | 2015-04-08 | 江门市优巨新材料有限公司 | Special material for high-fluidity high-temperature polyamide heat-insulation strip and preparation method of material |
| CN109776349A (en) * | 2017-11-15 | 2019-05-21 | 财团法人工业技术研究院 | Diamine compound, diamine diacid salt, the forming method with copolymer |
| CN112920400A (en) * | 2020-12-29 | 2021-06-08 | 深圳市华盈新材料有限公司 | Bio-based semi-aromatic polyamide copolymer and preparation method, composition and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104497569A (en) * | 2014-12-17 | 2015-04-08 | 江门市优巨新材料有限公司 | Special material for high-fluidity high-temperature polyamide heat-insulation strip and preparation method of material |
| CN104497569B (en) * | 2014-12-17 | 2017-04-12 | 江门市优巨新材料有限公司 | Special material for high-fluidity high-temperature polyamide heat-insulation strip and preparation method of material |
| CN109776349A (en) * | 2017-11-15 | 2019-05-21 | 财团法人工业技术研究院 | Diamine compound, diamine diacid salt, the forming method with copolymer |
| CN109776349B (en) * | 2017-11-15 | 2022-02-22 | 财团法人工业技术研究院 | Diamine compound, diamine diacid salt, and method for forming copolymer |
| CN112920400A (en) * | 2020-12-29 | 2021-06-08 | 深圳市华盈新材料有限公司 | Bio-based semi-aromatic polyamide copolymer and preparation method, composition and application thereof |
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| Publication number | Publication date |
|---|---|
| CN103012777B (en) | 2016-01-06 |
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