CN101870798B - Epoxy resin dough moulding compound and preparation method thereof - Google Patents
Epoxy resin dough moulding compound and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an epoxy resin dough moulding compound and a preparation method thereof. The epoxy resin dough moulding compound is prepared by evenly kneading 35-40 parts by mass of epoxy resin paste, 4-5 parts by mass of curing agent mixture and 65-70 parts by mass of chopped fiber, wherein the epoxy resin paste comprises the following components in parts by mass: 80-120 parts of epoxy resin, 5-10 parts of plasticizer, 4-8 parts of filler, 3-6 parts of mould release agent and 0.5-2 part(s) of coupling agent; the curing agent mixture comprises the following components in parts by mass: 4-7 parts of latent curing agent, 1-3 part(s) of accelerator and 6-10 parts of amine curing agent, and the length of the chopper fiber is one eighth to one half inch. Compared with the traditional method, the preparation method eliminates the curing process, and the dough moulding compound is prepared by adding modifying components and different curing systems into the epoxy resin. The method has the advantages of simple operation, high production efficiency, long working life and easy formation. Since the baking oven and other heating equipment are not needed, the method can reduce the energy consumption. Moreover, the method is applicable to fields of structural materials and composite materials with high requirements for insulation and electrical properties, and can be easily promoted and implemented.
Description
Technical field
The present invention relates to a kind of epoxy resin dough moulding compound and preparation method thereof.
Background technology
The moulding compound technology is a kind of sophisticated composite technology, and it has the advantages that by resin and blending in of fibers are evenly used the back quality is uniform and stable, shaping speed is fast, production efficiency is high.Common moulding compound mainly uses vibrin as resin matrix, have characteristics such as cost is low, solidification value is low, use the resin matrix of Resins, epoxy as moulding compound, have special advantages in some special technique field, as require long shelf lives, high second-order transition temperature, field such as mechanical property and electric property preferably.
Use Resins, epoxy less as the prescription of moulding compound raw material at present, all adopt the curing system of latent, need mostly could use after the slaking, technology is comparatively complicated; As publication number is the preparation method that the Chinese patent application of CN101096443A discloses a kind of Resins, epoxy sheet moulding compound, be with after the epoxy paste preparation, after the adding chopped strand mixes, make sheet material by scraper again, then through baking oven thickening slaking in 24-96 hour, the control thickening temperature is 28-40 ℃, obtains Resins, epoxy sheet moulding compound.The curing step operation that in the preparation of existing epoxy molding material, is absolutely necessary, during its consumption energy consumption, not easy to operate and production efficiency is low.
Summary of the invention
In order to solve the defective that exists in the above-mentioned prior art, the object of the present invention is to provide a kind of slaking, simple, the easy handling of technology, epoxy resin dough moulding compound that production efficiency is high and preparation method thereof of need not.
To achieve these goals, the present invention adopts following technical scheme: a kind of epoxy resin dough moulding compound, its characteristics are: it by epoxy paste, solidifying agent compound and chopped strand with 35～40: 4～5: 65～70 ratio of quality and the number of copies is mediated and is evenly formed; Wherein: epoxy paste contains 80～120 parts of Resins, epoxy according to the mass fraction, softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part; The solidifying agent compound contains latent curing agent 4-7 part according to the mass fraction, promotor 1-3 part, amine curing agent 6-10 part; The length of chopped strand is 1/8 inch～1/2 inch.
Resins, epoxy in the above-mentioned epoxy paste can be selected in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, glycidyl amine Resins, epoxy, ethylene oxidic ester epoxy resin and the alicyclic ring epoxide resin composition of any one or two kinds for use;
Above-mentioned softening agent can be selected in polyvinyl butyral acetal, dimethyl phthalate, diethyl phthalate or the dibutyl phthalate any for use;
The filler that adds in epoxy paste can be selected commercially available conventional packing for use, can select in silicon-dioxide, lime carbonate, aluminium hydroxide or the aluminum oxide any for use; The releasing agent that adds comprises resin with inorganic or organic inner pattern releasing agent applicable, can select in montanin wax, silicone grease or the Zinic stearas any for use; The coupling agent that adds is selected silane series coupling agent for use, and this silane series coupling agent can be selected for use: in KH550 silane coupling agent, KH560 silane coupling agent or the KH570 silane coupling agent any; The silane series coupling agent role is to improve the wettability of epoxy-resin systems, makes the splicing face over-all properties of formation better.
Amine curing agent in the above-mentioned solidifying agent compound can be selected in quadrol, diethylenetriamine, triethylene tetramine, isophorone diamine or the polyetheramine any for use; Latent curing agent can be selected common double cyanamide or electronic-grade Dyhard RU 100 for use; Promotor is selected N, N-dimethyl diphenyl urea or N, N-diethyl diphenyl urea for use; The collaborative use of two kinds of solidifying agent and a kind of promotor can make epoxy-resin systems have the viscosity and the curing process performance of expectation.
Above-mentioned chopped strand can be according to the purposes and the service requirements of product, selects in glass fibre, carbon fiber, aramid fiber or the silica fiber any for use, preferentially uses short glass fiber.
To achieve these goals, the present invention also provides a kind of method for preparing above-mentioned epoxy resin dough moulding compound, comprises that step is as follows:
1) preparation epoxy paste;
2) amine curing agent and latent curing agent are stirred after, add promotor again and stir into behind the solidifying agent compound standby;
3) get epoxy paste 35-40 mass parts, the step 2 of step 1)) the solidifying agent compound 4-5 mass parts and the chopped strand of 65～70 mass parts mediate by kneader and obtain described epoxy resin dough moulding compound after 30 minutes.
Wherein: the described epoxy paste of step 1) is included in and adds softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part in 80～120 parts of Resins, epoxy in proportion, mixes through high-speed stirring and makes; Step 2) described solidifying agent compound is add latent curing agent 4-7 part mixing and stirring in the amine curing agent of 6-10 part after, adds promotor 1-3 part again and continues to stir and make; The used chopped strand length of step 3) is 1/8 inch～1/2 inch.
The selection and the umber of above-mentioned Resins, epoxy, softening agent, filler, releasing agent, coupling agent material therefor, the selection of amine curing agent, latent curing agent and promotor material therefor and the selection of umber and chopped strand and length repeat no more all as previously mentioned herein.
The present invention has adopted technique scheme, and its beneficial effect is as follows: 1) by to the formulating of recipe of epoxy molding material, the collaborative use of several solidifying agent, prepare a kind of tack-free in room temperature environment, hard crisp moulding compound resin system under the low temperature; This resin system does not need to cool off pulverizing, need not slaking after directly Bulk Molding Compound is prepared in kneading with chopped strand yet, has saved the maturation stage that must need in the traditional method, compares with traditional method, and technology is simple, the production efficiency height; 2) because the adding of softening agent makes this epoxy molding material have excellent technology and mechanical property, tensile strength reaches more than the 160MPa.3) grow working life, be easy to moulding, need not use heating installations such as baking oven because of it, also have energy-saving and cost-reducing effect, be easy to promotion and implementation.
Embodiment
Epoxy resin dough moulding compound of the present invention, by epoxy paste, solidifying agent compound and chopped strand with 35～40: 4～5: 65～70 ratio of quality and the number of copies is mediated and is evenly formed; Wherein: epoxy paste contains 80～120 parts of Resins, epoxy according to the mass fraction, softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part; The solidifying agent compound contains latent curing agent 4-7 part according to the mass fraction, promotor 1-3 part, amine curing agent 6-10 part; The length of chopped strand is 1/8 inch～1/2 inch.
For making moulding compound have good materialization, mechanical property, above-mentioned Resins, epoxy can be selected in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, glycidyl amine Resins, epoxy, ethylene oxidic ester epoxy resin and the alicyclic ring epoxide resin composition of any one or two kinds for use;
Above-mentioned softening agent can be selected in polyvinyl butyral acetal, dimethyl phthalate, diethyl phthalate or the dibutyl phthalate any for use; The adding of softening agent has reduced the potential barrier of chain movement between this cured resin system cross-linking set, has given this epoxy-resin systems better processability and bigger snappiness.
Above-mentioned filler can be selected commercially available mineral filler for use, and the best can be selected in silicon-dioxide, lime carbonate, aluminium hydroxide or the aluminum oxide any for use; The use of mineral filler, its effect are the viscosity that increases described epoxy paste, reduce cost, reduce the goods shrinking percentage.
Above-mentioned releasing agent comprises resin with inorganic releasing agent or organic inner pattern releasing agent applicable, can select in montanin wax, silicone grease or the Zinic stearas any for use, and using the effect of releasing agent is to make the easy demoulding of goods, guarantees the visual appearance of its goods.
Above-mentioned coupling agent adopts silane series coupling agent, can select for use: in KH550 silane coupling agent, KH560 silane coupling agent or the KH570 silane coupling agent any; The silane series coupling agent role is to improve the wettability of epoxy-resin systems, makes the cement plane over-all properties of formation better.
Above-mentioned amine curing agent can be selected in quadrol, diethylenetriamine, triethylene tetramine, isophorone diamine or the polyetheramine any for use; Latent curing agent can be selected common double cyanamide or electronic-grade Dyhard RU 100 for use; Promotor is selected N, N-dimethyl diphenyl urea or N, N-diethyl diphenyl urea for use; The collaborative use of two kinds of solidifying agent and a kind of promotor can make epoxy-resin systems have the viscosity and the curing process performance of expectation.
Above-mentioned chopped strand can be according to the purposes and the service requirements of product, selects in glass fibre, carbon fiber, aramid fiber or the silica fiber any for use, preferentially uses short glass fiber.
Second purpose of the present invention provided a kind of method for preparing above-mentioned epoxy resin dough moulding compound, comprises that step is as follows:
1) preparation epoxy paste;
2) amine curing agent and latent curing agent are stirred after, add promotor again and stir into behind the solidifying agent compound standby;
3) get epoxy paste 35-40 mass parts, the step 2 of step 1)) the solidifying agent compound 4-5 mass parts and the chopped strand of 65～70 mass parts mediate by kneader and obtain described epoxy resin dough moulding compound after 30 minutes.
Wherein: the described epoxy paste of step 1) is included in and adds softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part in 80～120 parts of Resins, epoxy in proportion, mixes through high-speed stirring and makes; Step 2) described solidifying agent compound is add latent curing agent 4-7 part mixing and stirring in the amine curing agent of 6-10 part after, adds promotor 1-3 part again and continues to stir and make; The used chopped strand length of step 3) is 1/8 inch～1/2 inch.
This preparation method has improved the prescription of epoxy paste, and solidifying agent adopts the collaborative use of plurality of raw materials, and the adding of chopped strand, makes the preparation method of epoxy resin dough moulding compound more simple and direct; Simultaneously, raw materials usedly need not cool off pulverizing, can directly mediate with chopped strand and form the Bulk Molding Compound goods, save the maturation stage that must need in the traditional technology, improve production efficiency; Compare with traditional method, technology is simple, has saved production cost, has reduced energy consumption, and is time saving and energy saving.
Below by specific embodiment technical scheme of the present invention is described in further detail.
Except as otherwise noted, the used various raw materials of following examples all can obtain by commercial sources.Used umber is all represented mass parts.
Example 1
Prepare earlier epoxy paste, solidifying agent compound respectively, and selected used chopped strand; Wherein:
It is 80 parts of the liquid bisphenol A type epoxy resins of WSR618 that epoxy paste is selected model for use, 5 parts of dimethyl phthalates, 4 parts of silicon-dioxide, 3 parts of montanin waxs, 0.5 part of coupling agent KH550, be fed in the homogenizer, this homogenizer is standby after 0.5 hour with 800 rev/mins speed stirring; The model that homogenizer selects for use German IKA company to produce is: RW 20 DZM stirrers.
10 parts of isophorone diamines are selected in the preparation of solidifying agent compound earlier for use, add therein after 4 parts of common double cyanamides stir, and adding 1 part of N, N-dimethyl diphenyl urea again, to continue to mix the back standby.
Chopped strand is selected 1/4 cun short glass fiber for use.
The preparation method of epoxy resin dough moulding compound of the present invention: 35 parts of extracting epoxy resin pastes, 5 parts of solidifying agent compounds, short glass fiber pass through this kneader for 65 parts to be mixed after 30 minutes, can obtain this epoxy resin dough moulding compound; This Bulk Molding Compound can be used for packaged material of suppressing electric insulation device, unicircuit etc.
This example 1 properties of sample testing method and the results are shown in Table 1.
Example 2:
Prepare earlier epoxy paste, solidifying agent compound respectively, and selected used chopped strand; Wherein:
Select 110 parts of Resins, epoxy in the epoxy paste for use, contain model in this Resins, epoxy and be 50 parts of 60 parts of the liquid bisphenol A type epoxy resins of WSR618 and bisphenol F epoxy resin resins that model is ADK4901; Softening agent is selected 7 parts of polyvinyl butyral acetals for use, and filler is selected 5 parts in lime carbonate for use, and releasing agent is selected 4 parts of silicone grease for use, and coupling agent is selected 1 part of KH560 for use.
The amine curing agent that contains in the solidifying agent compound is selected 6 parts of quadrols for use, and latent curing agent is selected 7 parts of electronic-grade Dyhard RU 100s for use, and promotor is selected 2 parts of N, N-dimethyl diphenyl ureas for use;
Chopped strand is selected 1/2 cun chopped carbon fiber for use.
35 parts of extracting epoxy resin pastes, 5 parts of solidifying agent compounds during use, chopped strand 65 is fed in the kneader, mixes after 30 minutes, makes epoxy resin dough moulding compound of the present invention.This Bulk Molding Compound can be used for packaged material of suppressing electric insulation device, unicircuit etc.
Properties of sample testing method and the results are shown in Table 1.
Example 3
Prepare earlier epoxy paste, solidifying agent compound respectively, and selected used chopped strand; Wherein:
Contain 120 parts of Resins, epoxy in the epoxy paste, comprising 60 parts of models be WSR618 liquid bisphenol A type epoxy resin and 60 parts of ethylene oxidic ester epoxy resins that model is TDE-85, softening agent is selected 10 parts of diethyl phthalates for use, filler is selected 8 parts in aluminium hydroxide for use, releasing agent is selected 6 parts of Zinic stearass for use, and coupling agent is selected 2 parts of KH560 silane coupling agents for use.
Contain amine curing agent in the solidifying agent compound and select 7 parts of diethylenetriamines for use, latent curing agent is selected 7 parts of electronic-grade Dyhard RU 100s for use, and promotor is used 3 parts of N, N-diethyl diphenyl ureas.
It is that 1/8 cun weak point is cut aramid fiber that chopped strand is selected for use.
35 parts of extracting epoxy resin pastes, 5 parts of solidifying agent mixing, weak point are cut 70 parts of aramid fibers during use, are fed in the kneader, mix after 30 minutes, make epoxy resin dough moulding compound of the present invention.This epoxy resin dough moulding compound can be used for packaged material of suppressing electric insulation device, unicircuit etc.
Its properties of sample testing method and the results are shown in Table 1.
Except that above-mentioned example, Resins, epoxy used in the epoxy paste also can be selected glycidyl amine Resins, epoxy and alicyclic ring epoxide resin for use; Softening agent also can be selected dibutyl phthalate for use; Amine curing agent can also be selected triethylene tetramine, polyetheramine for use; Filler also can be selected aluminum oxide for use, and chopped strand also can be selected silica fiber etc. for use.
The used test set of properties of sample test in the above-mentioned example of the present invention is that the mechanical test machine of routine and the model of U.S. TA company production are the dynamic thermal analysis instrument of DMA2980.
Table 1
| Test event | Testing method | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Tensile strength/MPa | GB1447-2005 | 161 | 202 | 185 |
| Fail in tension load/KN | GB1447-2005 | 10.25 | 14.05 | 13.16 |
| Shelf lives (less than 10 ℃)/moon | Store back repetition measurement intensity in the refrigerator | 3 | 3 | 3 |
| Second-order transition temperature/℃ | Use the test of dynamic thermal analysis instrument | 120 | 125 | 120 |
Claims (7)
1. epoxy resin dough moulding compound is characterized in that: it by epoxy paste, solidifying agent compound and chopped strand with 35～40: 4～5: 65～70 ratio of quality and the number of copies is mediated and is evenly formed; Wherein: epoxy paste contains 80～120 parts of Resins, epoxy according to the mass fraction, softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part; The solidifying agent compound contains latent curing agent 4-7 part according to the mass fraction, promotor 1-3 part, amine curing agent 6-10 part; The length of chopped strand is 1/8 inch～1/2 inch; Wherein, described latent curing agent be in common double cyanamide or the electronic-grade Dyhard RU 100 any; Described promotor be in N, N-dimethyl diphenyl urea or N, the N-diethyl diphenyl urea any; Described amine curing agent is selected in quadrol, diethylenetriamine, triethylene tetramine, isophorone diamine or the polyetheramine any for use.
2. epoxy resin dough moulding compound according to claim 1 is characterized in that: described Resins, epoxy is selected any one or two kinds of combination in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, glycidyl amine Resins, epoxy, ethylene oxidic ester epoxy resin and the alicyclic ring epoxide resin for use.
3. epoxy resin dough moulding compound according to claim 1 is characterized in that: described softening agent is selected in polyvinyl butyral acetal, dimethyl phthalate, diethyl phthalate or the dibutyl phthalate any for use.
4. epoxy resin dough moulding compound according to claim 1 is characterized in that: described releasing agent be in montanin wax, silicone grease or the Zinic stearas any; Described coupling agent be in KH550 silane coupling agent, KH560 silane coupling agent or the KH570 silane coupling agent any.
5. epoxy molding material according to claim 1 is characterized in that: described chopped strand be in glass fibre, carbon fiber, aramid fiber or the silica fiber any.
6. the preparation method of an epoxy resin dough moulding compound comprises the steps:
1) preparation epoxy paste;
2) get amine curing agent and latent curing agent and stir after, add promotor again and stir into behind the solidifying agent compound standby;
3) get epoxy paste 35-40 mass parts, the step 2 of step 1)) the solidifying agent compound 4-5 mass parts and the chopped strand of 65～70 mass parts mediate by kneader and obtain described epoxy resin dough moulding compound after 30 minutes;
Wherein: the described epoxy paste of step 1) is included in and adds softening agent 5-10 part, filler 4-8 part, releasing agent 3-6 part, coupling agent 0.5-2 part in 80～120 parts of Resins, epoxy in proportion, mixes through high-speed stirring and makes; Step 2) described solidifying agent compound is add latent curing agent 4-7 part mixing and stirring in the amine curing agent of 6-10 part after, adds promotor 1-3 part again and continues to stir and make; Wherein, described amine curing agent is selected in quadrol, diethylenetriamine, triethylene tetramine, isophorone diamine or the polyetheramine any for use; Latent curing agent be in common double cyanamide or the electronic-grade Dyhard RU 100 any; Described promotor be in N, N-dimethyl diphenyl urea or N, the N-diethyl diphenyl urea any; The used chopped strand length of step 3) is 1/8 inch～1/2 inch.
7. preparation method according to claim 6 is characterized in that: described Resins, epoxy is selected any one or two kinds of combination in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, glycidyl amine Resins, epoxy, ethylene oxidic ester epoxy resin, the alicyclic ring epoxide resin for use; Described softening agent is selected in polyvinyl butyral acetal, dimethyl phthalate, diethyl phthalate or the dibutyl phthalate any for use; Described releasing agent is selected in montanin wax, silicone grease or the Zinic stearas any for use; Described coupling agent be in KH550 silane coupling agent, KH560 silane coupling agent or the KH570 silane coupling agent any; Described chopped strand be in glass fibre, carbon fiber, aramid fiber or the silica fiber any.
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