CN101585958B - Composition and method for preparing artificial gem - Google Patents
Composition and method for preparing artificial gem Download PDFInfo
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- CN101585958B CN101585958B CN2009100405613A CN200910040561A CN101585958B CN 101585958 B CN101585958 B CN 101585958B CN 2009100405613 A CN2009100405613 A CN 2009100405613A CN 200910040561 A CN200910040561 A CN 200910040561A CN 101585958 B CN101585958 B CN 101585958B
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Abstract
The present invention provides a combination for preparing an artificial gem, composed of 100 weight shares of a resin component and 25-50 weight shares of a solidify component; wherein said resin component is prepared by the following method: fetching 70-80 weight shares of bisphenol F glycidyl ether, 10-20 weight shares of bisphenol F epoxy resin and 5-10 weight shares of reactive diluent to mix, heating until 40-60 DEG C, agitating to react for one to two hours, and cooling to a room temperature; the solidify component is prepared by the following method: (1) fetching 10-20 weight shares ofnon reactive diluent, 15-25 weight shares of aliphatic amine and 20-40 weight shares of alicyclic ring amine to mix, heating until 50-60 DEG C, (2) adding 10-20 weight shares of reactive diluent slow ly when agitating, then elevating the temperature to 80 DEG C, heat preserving for one to two hours, (3) cooling to 40 DEG C, adding 10-20 weight shares of polyetheramine, agitating until non precipitation, then cooling to the room temperature.
Description
Technical field
The present invention relates to chemical field, being specifically related to the organic high molecular compound is the composition of base-material.
Background technology
Jewel because beautiful, hard, rare and in commodity exchange quilt tax with very high value.Natural gemstone be from the rock of occurring in nature through excavating exploitation, high-temperature calcination roughing is further refined after the precision work cutting again and is burnished and fabricated and form.But the jewel rareness of occurring in nature can not satisfy people's demand far away.
In order to satisfy people's demand, hard mass arises at the historic moment.Hard mass divides two classes: a kind of is synthetic gem, and this series products has identical Chemical Composition, crystalline structure and physical properties with corresponding natural gemstone; Another kind is the imitation or the surrogate of jewel, is meant with natural gemstone to have similar in appearance or optical effect, but does not possess the Chemical Composition of natural gemstone, the material of crystalline structure.Yet, want synthetic a kind of product existing technical still very difficult, and utilize relatively easy and cheap many of the imitation of other material preparation with the chemical ingredients identical, crystalline structure and physical properties with natural gemstone.
The material that is used to prepare the jewel imitation at present mainly is a Resins, epoxy, know a patent of invention " a kind of hard transparent epoxy resin-base composite material and synthetic method thereof " (Granted publication CN1180022C) of Granted publication on the 15th in office's December in 2004 as state, this patent disclosure a kind of synthetic method of hard transparent epoxy resin-base composite material, this method is made up of following steps: (1) gets solidifying agent with 20～30 weight part solidifying agent saturated hydrocarbyl monoamines and/or-oxyl monoamine distillation removing oxydised component; (2) 100 weight part Resins, epoxy and 6～9 weight part properties-correcting agent O-phthalic bases different monooctyl ester of acid and/or n-butyl phthalate are mixed; (3) in the mixture that the slow implantation step of solidifying agent (2) after step (1) distillation is obtained simultaneously orientation stir to clarify transparently, leave standstill curing under the normal temperature.The gained hard transparent epoxy resin-base composite material is sparkling and crystal-clear transparent, and shrinking percentage is little, and machining property is good, and chemical property is stable, can be used for processing various furniture and ornament.But the present most poor mechanical property of resene hard mass on sale on the market, and easily moisture absorption or oxidizedly cause opaque, the jaundice in surface cause optical property to descend.
Summary of the invention
The problem to be solved in the present invention is to solve transparency and the mechanical property that improves the epoxy resin hard mass.
The technical scheme that the present invention addresses the above problem is:
A kind of composition for preparing hard mass, said composition is made up of the resin Composition of 100 weight parts and the curing component of 25～50 weight parts; Wherein,
Described resin Composition is mainly prepared by following method: get the Bisphenol F glycidyl ether (for example EPON-862 Resins, epoxy of Shell Co. Ltd) of 70～80 weight parts, the bisphenol F epoxy resin of 10～20 weight parts and the reactive thinner of 5～10 weight parts and mix, be heated to 40～60 ℃, stirring reaction 1～2 hour is cooled to room temperature;
Described curing component is mainly prepared by following method: (1) gets the non-activated thinner of 10～20 weight parts, and the aliphatic cyclic amine of the aliphatic amide of 15～25 weight parts and 20～40 weight parts mixes, and is heated to 50～60 ℃; (2) slowly add 10～20 weight part reactive thinners while stirring, be warming up to 80 ℃ then, be incubated 1～2 hour; (3) reduce to 40 ℃, add the polyetheramine of 10～20 weight parts, be stirred to no post precipitation cool to room temperature;
Among the preparation method of above-mentioned resin Composition and curing component, described reactive thinner is the ether material that contains bis-epoxy functional group, as ethylene glycol diglycidylether, propylene glycol diglycidylether or butanediol diglycidyl ether; Described aliphatic amide is diethylenetriamine, Triethylenetetramine (TETA) or an xylidine; Described aliphatic cyclic amine is isophorone diamine, N-aminoethyl piperazine, 4,4 '-diamino-dicyclohexyl methane, 3,3 '-dimethyl-4,4 '-diamino-dicyclohexyl methane, 2,2-two (4-aminocyclohexyl) propane or 2,2-two (3-methyl-4-aminocyclohexyl) propane; Described polyetheramine is to be the diamines or the triamine (for example D230, D400, T403 etc.) of main chain with polyethylene oxide or propylene oxide; Described non-activated thinner is dibutyl phthalate, dioctyl phthalate (DOP), phenylcarbinol or propyl carbinol.
The present composition, the consumption of Bisphenol F glycidyl ether, bisphenol F epoxy resin, reactive thinner that is used to prepare described resin Composition is preferred: Bisphenol F glycidyl ether 80 weight parts, bisphenol F epoxy resin 10 weight parts, reactive thinner 5 weight parts; The consumption of aliphatic amide, aliphatic cyclic amine and reactive thinner that is used to prepare described curing component is preferred: non-activated thinner 15 weight parts, aliphatic amide 15 weight parts, aliphatic cyclic amine 35 weight parts and reactive thinner 25 weight parts.
The present composition, the preparation method of wherein said resin Composition, when getting Bisphenol F glycidyl ether, bisphenol F epoxy resin and reactive thinner mixing, the non-activated thinner that can also get 5～10 weight parts mixes together, in order to reduce the viscosity of system; Described non-activated thinner is dibutyl phthalate, dioctyl phthalate (DOP), phenylcarbinol or propyl carbinol, preferred 15 weight parts of consumption.
The present composition, can also add various auxiliary agents in the preparation process of wherein said resin Composition, to obtain better effect, as add the bubble that defoamer can be eliminated the cured article surface, add flow agent and can make the surface of cured article more smoothly glossy, add dispersion agent cured article is uniformly dispersed.
The present composition, in the preparation process of wherein said curing component (1), when getting non-activated thinner, aliphatic amide and aliphatic cyclic amine mixing, the curing catalyst that can also get 15～25 weight parts mixes together, make the epoxy group(ing) etherificate in the Bisphenol F glycidyl ether, accelerate epoxy group(ing) and amino speed of response; Described curing catalyst is a hydroxy-benzoic acid, 2,4,6-three (dimethylamino methyl) phenol, nonyl phenol, dihydroxyphenyl propane or cardanol, preferred 10 weight parts of consumption.
The preparation method of the present composition is: described resin Composition and curing component are mixed by proportioning get final product.
Composition of the present invention can be used for preparing hard mass, its method mainly is made up of following steps: with the present composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, can obtain a kind of water white hard solid.When preparing hard mass, the mill base (also can determine color paste consumption) of described composition weight 1～3% can also be added, and then the hard mass of different colours can be obtained by the above-mentioned steps preparation according to concrete needs with the present composition.
The hard mass of aforesaid method gained, testing its second-order transition temperature (Tg) through the differential thermal analyzer of CDR-1 type (DSC) is 110～120 ℃, the hardness of testing under its 25 ℃ through Shao's formula sclerometer is 85～90, and the tensile strength of testing under its 25 ℃ through LJ-500 type pulling experiment machine is 11～12Mpa.
Resin Composition in the composition of the present invention and curing component consistency are fine, and the high molecular polymer solid (reaction process is seen formula I) that polyaddition reaction generates hard, clear can take place under the certain temperature condition.Gained solid phase prod water white transparency, cure shrinkage and coefficient of linear expansion are little, mechanical property, dielectric properties and excellent anti-corrosion performance, not only can compare favourably with natural gemstone, also solve the shortcoming that existing epoxy resin hard mass surface is opaque and turn to be yellow in color, outward appearance, optical effect and use properties.
Cause that the opaque reason in hard mass surface is that part active amino in the amine curing agent produces the carbonic acid amine salt with airborne water and carbon dioxide reaction easily, the reason that causes jaundice is a lot of but most important reason is the oxidized production quinone of the phenol structure structure in the amine curing agent.The present invention adopts the bis-epoxy reactive thinner to react with these active groups in advance, can effectively avoid the influence to hard mass of water, carbonic acid gas and oxygen, has also improved the consistency of two kinds of components simultaneously.
Embodiment
Example 1
1, the present composition is that 2: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the n-butyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 10g and the isophorone diamine of 55g in reactor, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
The gained solid is prepared into sample according to the requirement of standard GB 1039-1043-79 plastics mechanical test method, testing its second-order transition temperature (Tg) through the differential thermal analyzer of CDR-1 type (DSC) is 110 ℃, the hardness of testing under its 25 ℃ through Shao's formula sclerometer is 85, and the tensile strength of testing under its 25 ℃ through LJ-500 type pulling experiment machine is 10.8Mpa.
Example 2
1, the present composition is that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 75g and the EPON-862 Resins, epoxy of 15g in reactor, be heated to 60 ℃, add the phenylcarbinol of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: in reactor, add the dibutyl phthalate of 10g and 50g between xylidine, be warmed up to 60 ℃, slowly add butanediol diglycidyl ether 15g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ again, add 20g polyetheramine D230 and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
The gained solid is prepared into sample according to the requirement of standard GB 1039-1043-79 plastics mechanical test method, testing its second-order transition temperature (Tg) through the differential thermal analyzer of CDR-1 type (DSC) is 112 ℃, the hardness of testing under its 25 ℃ through Shao's formula sclerometer is 88, and the tensile strength of testing under its 25 ℃ through LJ-500 type pulling experiment machine is 11.6Mpa.
Example 3
1, the present composition is that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 20g and the dihydroxyphenyl propane of 10g in reactor, be warming up to 60 ℃, add 4 of 40g, 4 '-two amidos, two cyclohexyl methanes, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
The gained solid is prepared into sample according to the requirement of standard GB 1039-1043-79 plastics mechanical test method, testing its second-order transition temperature (Tg) through the differential thermal analyzer of CDR-1 type (DSC) is 115 ℃, the hardness of testing under its 25 ℃ through Shao's formula sclerometer is 85, and the tensile strength of testing under its 25 ℃ through LJ-500 type pulling experiment machine is 12Mpa.
Example 4
1, the present composition is that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the phenylcarbinol of 5g and the butylglycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, the isophorone diamine of 35g, be warmed up to 60 ℃, slowly add ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
The gained solid is prepared into sample according to the requirement of standard GB 1039-1043-79 plastics mechanical test method, testing its second-order transition temperature (Tg) through the differential thermal analyzer of CDR-1 type (DSC) is 120 ℃, the hardness of testing under its 25 ℃ through Shao's formula sclerometer is 92, and the tensile strength of testing under its 25 ℃ through LJ-500 type pulling experiment machine is 12.5Mpa.
Example 5
1, the present composition is that 4: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the phenyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 10g and the N-aminoethyl piperazine of 55g in reactor, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 6
1, the present composition is that 3: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the lauryl diglycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add 4 of the phenylcarbinol of 10g and 55g in reactor, 4 '-diamino-dicyclohexyl methane, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 7
1, the present composition is that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 10g and the ortho-cresol glycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 3 of 35g, 3 '-dimethyl-4,4 '-diamino-dicyclohexyl methane, be warmed up to 60 ℃, slowly add ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 8
1, the present composition is that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 10g and the ortho-cresol glycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 2 of 35g, 2-two (4-aminocyclohexyl) propane is warmed up to 60 ℃, slowly adds ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 9
1, the present composition is that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 2g and the propyl carbinol of 8g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 2 of 35g, 2-two (3-methyl-4-aminocyclohexyl) propane is warmed up to 60 ℃, slowly adds ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 10
1, the present composition is that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add 2 of the phenylcarbinol of 20g and 20g in reactor, 4,6-three (dimethylamino methyl) phenol is warming up to 60 ℃, adds 4 of 40g, 4 '-two amidos, two cyclohexyl methanes, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 11
1, the present composition is that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 20g and the hydroxy-benzoic acid of 10g in reactor, be warming up to 60 ℃, add 4 of 40g, 4 '-two amidos, two cyclohexyl methanes, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Example 12
1, the present composition is that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 20g and the cardanol of 15g in reactor, be warming up to 60 ℃, add 4 of 40g, 4 '-two amidos, two cyclohexyl methanes, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
2, the preparation of the artificial jewel of the present invention: with above-mentioned composition be cast to mould leave standstill do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
Comparative Examples
1, commercially available hard mass 101 is available from the prosperous chemical industry in Dongguan company limited.
2, performance test:
(1) external inspection.
(2) the said products is prepared into sample according to the requirement of standard GB 1039-1043-79 plastics mechanical test method, use the differential thermal analyzer of CDR-1 type (DSC) to test its second-order transition temperature (Tg) then, test hardness under its 25 ℃ with Shao's formula sclerometer, test tensile strength under its 25 ℃ with LJ-500 type pulling experiment machine.
The jaundice of this hard mass surface, transparency is not high, and every The performance test results is as follows: second-order transition temperature is 65 ℃, and the hardness under 25 ℃ is that the tensile strength under 82,25 ℃ is 9.4Mpa.From The above results as can be seen, the outward appearance of commercially available prod and every performance all prepare the product of gained not as the present composition.
Claims (2)
1. composition for preparing hard mass, said composition is one of following (1)～(12):
(1) be that 2: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the n-butyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 10g and the isophorone diamine of 55g in reactor, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
(2) be that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 75g and the EPON-862 Resins, epoxy of 15g in reactor, be heated to 60 ℃, add the phenylcarbinol of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: in reactor, add the dibutyl phthalate of 10g and 50g between xylidine, be warmed up to 60 ℃, slowly add butanediol diglycidyl ether 15g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ again, add 20g polyetheramine D230 and stir, be cooled to the room temperature discharging at last and get curing component;
(3) be that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 20g and the dihydroxyphenyl propane of 10g in reactor, be warming up to 60 ℃, add 4 of 40g, 4 '-two amidos, two cyclohexyl methanes, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
(4) be that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the phenylcarbinol of 5g and the butylglycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, the isophorone diamine of 35g, be warmed up to 60 ℃, slowly add ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
(5) be that 4: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the phenyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 10g and the N-aminoethyl piperazine of 55g in reactor, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
(6) be that 3: 1 resin Composition and curing component formed by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the lauryl diglycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add 4 of the phenylcarbinol of 10g and 55g in reactor, 4 '-diamino-dicyclohexyl methane, be warmed up to 50 ℃, slowly add ethylene glycol diglycidylether 15g while stirring, be warmed up to 80 ℃ then, react and cool to 40 ℃ after 2 hours, add 20g polyetheramine T403 and stir, be cooled to the room temperature discharging at last and get curing component;
(7) be that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 10g and the ortho-cresol glycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 3 of 35g, 3 '-dimethyl-4,4 '-diamino-dicyclohexyl methane, be warmed up to 60 ℃, slowly add ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
(8) be that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 10g and the ortho-cresol glycidyl ether of 5g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 2 of 35g, 2-two (4-aminocyclohexyl) propane is warmed up to 60 ℃, slowly adds ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
(9) be that 2: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 80g and the EPON-862 Resins, epoxy of 10g in reactor, be heated to 60 ℃, add the dioctyl phthalate (DOP) of 2g and the propyl carbinol of 8g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: the phenylcarbinol that adds 15g in reactor, xylidine between 15g, 2 of 35g, 2-two (3-methyl-4-aminocyclohexyl) propane is warmed up to 60 ℃, slowly adds ethylene glycol diglycidylether 25g while stirring, be warmed up to 80 ℃ of reactions 2 hours then, cool to 40 ℃ of nonyl phenols that add 10g, add 20g polyetheramine T403 to room temperature and stir, be cooled to the room temperature discharging at last and get curing component;
(10) be that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add 2 of the phenylcarbinol of 20g and 20g in reactor, 4,6-three (dimethylamino methyl) phenol is warming up to 60 ℃, adds 4 of 40g, 4 '-two amido dicyclohexyl methyl hydrides, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
(11) be that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: in reactor, add 20g phenylcarbinol and, the hydroxy-benzoic acid of 10g, be warming up to 60 ℃, 4,4 '-two amido dicyclohexyl methyl hydrides that add 40g stir after dissolving, add the 10g propylene glycol diglycidylether again, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component;
(12) be that 3: 1 resin Composition and curing component are mixed with and obtain by weight ratio; Wherein,
Resin Composition is prepared by following method: add the NPEL-128 Resins, epoxy of 70g and the EPON-862 Resins, epoxy of 20g in reactor, be heated to 60 ℃, add the phenmethyl glycidyl ether of 10g, stirred 30 minutes, cooling discharge obtains resin Composition;
Curing component is prepared by following method: add the phenylcarbinol of 20g and the cardanol of 15g in reactor, be warming up to 60 ℃, add 4 of 40g, 4 '-two amido dicyclohexyl methyl hydrides, stirring adds the 10g propylene glycol diglycidylether again after dissolving, be warmed up to 80 ℃ after adding again, stir and cool to 40 ℃ of polyetheramine D400 that add 20g again after 2 hours, be cooled to the room temperature discharging at last and get curing component.
2. the preparation method of an epoxy resin hard mass, this method is made up of following steps: with the described composition of claim 1 cast in leave standstill in the mould do not have bubble to the surface after, polyaddition reaction is 1.5 hours under 60 ℃ of conditions, obtains water white solid.
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| CN2009100405613A CN101585958B (en) | 2009-06-25 | 2009-06-25 | Composition and method for preparing artificial gem |
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| CN103304964A (en) * | 2013-06-17 | 2013-09-18 | 漳州丽都化工有限公司 | High-grade imitation jade material and preparation method thereof |
| WO2015077918A1 (en) | 2013-11-26 | 2015-06-04 | Dow Global Technologies Llc | Curing agent composition |
| CN104497275A (en) * | 2014-12-12 | 2015-04-08 | 宋良俊 | Modified aromatic amine epoxy curing agent and preparation method thereof |
| CN104403088A (en) * | 2014-12-12 | 2015-03-11 | 宋良俊 | Modified polyether amine epoxy curing agent and preparation method thereof |
| CN112048269A (en) * | 2020-08-18 | 2020-12-08 | 厦门坤信隆工贸有限公司 | Model machine coating adhesive and production process thereof |
| CN113214767B (en) * | 2021-05-08 | 2023-02-24 | 烟台大学 | Low-temperature high-hardness epoxy glue for metallographic cold embedding of heat sensitive element |
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