CN105295004A - High viscosity curing agent composition - Google Patents

Abstract

The invention discloses a high viscosity curing agent composition. Different types of curing agents are compounded for realizing higher bonding strength.

Description

A kind of high viscosity curing agent composition

Technical field

The present invention relates to a kind of high viscosity curing agent composition, particularly one and be applicable to the display element high viscosity curing agent compositions such as bonding liquid crystal.

Background technology

Solidifying agent has another name called stiffening agent, ripening agent or set agent, is that a class is promoted or controls material or the mixture of curing reaction.Resin solidification is through the chemical reactions such as condensation, closed loop, addition or catalysis, makes thermosetting resin that irreversible change procedure occur, and solidification has come by adding solidification (being cross-linked) agent.Solidifying agent is absolutely necessary additive, is to make caking agent, coating, mould material all to need to add solidifying agent, otherwise epoxy resin can not solidify.

In recent years, increase, the frame of the display part of adjoint liquid-crystal display are more and more narrow, and the graph thinning of sealing agent is advanced.In addition, as the adhering object of sealing agent, glass is not only by adhering object, also comprising inorganic materials, the alignment films etc. such as ITO electrode, SiN film organic materials etc. also becomes by adhering object, adherend becomes variation, the cementability variation requiring sealing agent to have foreign material can be bonded to each other.

This area faces main, is the requirement of various mobile phone and TV, indicating meter etc. and Rimless narrow to frame, and because its frame is more and more less, the fixing of display element device has just become a difficult problem.For the bonding way that this area is the most frequently used, more and more higher requirement is proposed to bonding strength.

But existing solidifying agent, most cohesive strength is inadequate, or can provide close cohesive strength, but cost is high, loses market-oriented meaning.

Summary of the invention

The object of the invention is to propose a kind of high viscosity curing agent composition, it is composite by dissimilar solidifying agent, provides the higher viscosity met the demands.

For reaching this object, the present invention by the following technical solutions:

A kind of curing agent composition, it comprises following component:

The mass ratio of two kinds of components described in described composition is 3:1-1:3, and preferred 2:1-1:2, has preferred 2:1 further.

Embodiment

The present invention is described high viscosity curing agent composition of the present invention by following embodiment.

Embodiment 1

I. the synthesis of formula 1 compound

Described in formula 1, compound is known compound, and those skilled in the art can obtain in commercially available purchase, also can synthesize and prepare.Its typical but non-limiting synthesis example is as follows:

Prepare in ethanol 150g, be dissolved with the lysate A of 1,12-diamino dodecane (manufacture of TCI society) 49.65g and in ethanol 118g, be dissolved with the lysate B of hexamethylene diisocyanate 20.54g.In there-necked flask, lysate B is controlled at 30 DEG C while stir, drip lysate A with the speed of 1.4g/ minute simultaneously.After dropping terminates, utilize Fourier Tranform infrared spectrophotometer assaying reaction liquid, confirm the 2250cm from isocyanate group ^-1termination reaction after neighbouring peak disappears.Reaction is there occurs according to the mode relative to hexamethylene diisocyanate 1 mole, 1,12-diamino dodecane being 2 moles (taking molar ratio computing as 1:2).

Thereafter, rotatory evaporator is utilized under reduced pressure to distill except desolventizing.Naturally cool to room temperature after drying, produce the compound of formula 1.

II. the synthesis of formula 2 compound

Described compound is known compound, and those skilled in the art can obtain in commercially available purchase, also can synthesize and prepare.Its typical but non-limiting synthesis example is as follows:

First prepare dinitrobenzene precursor.By the anti-form-1 of a part 28.44 grams, 2-diamino-cyclohexane is weighed in 1000 ml flasks together with 26.4 grams of triethylamines and 300 grams of chlorobenzenes.Under mechanical stirring, in room temperature with in 1 hour, add the 3-nitrobenzoyl chloride of 97 grams of powderies, and add chlorobenzene as required further to keep mobility.Mixture heat release to 30 DEG C.This mixture is cooled, filters, and with IMS and water washing.After 80 DEG C of dryings, obtain white powder, 71 grams, 69% yield, fusing point 266 DEG C.

The process preparing amine from above-mentioned dinitro compound is as follows.68 grams of dinitro compounds are added, the palladium/carbon (first soaking with the IMS of 50ml) of 250 milliliters of IMS and 2.7 gram 10% in the flask of 1 liter.Fully stir under nitrogen atmosphere, in 1 hour, then drip the hydrazine hydrate of 45 milliliters, be then warming up to 60 DEG C and keep 2 hours.Product is cooled, filters, with IMS and water washing.This crude solid is refined, is namely dissolved in warm dilute hydrochloric acid, then filter to remove carbon elimination.Flaxen filtrate neutralizes with ammonia soln, is then filtered by generated white solid, washes with water and vacuum-drying.Obtain white powder, yield 90% (52.3 grams), its fusing point is 274 ~ 276 DEG C.Described powder is compound shown in formula 2.。

By the component I for preparing and II, obtain described curing agent composition according to 2:1 is composite.

Preparation methacrylic acidylate epoxy resin 100 mass parts, spherical silicon dioxide 15 mass parts as inorganic filler, the F-351 as organic filler (Japanese Zeon society manufactures) 15 mass parts, Irgacure907 (BASF manufacture) 3 mass parts as optical free radical initiator, (manufacture of chemical industry society of SHIN-ETSU HANTOTAI) 2 mass parts of the KBM-403 as silane coupling agent and curing agent composition of the present invention 2 mass parts are carried out dispersed, obtain liquid crystal sealing agent composition.

Prepare the square ito glass of thickness 0.5mm, 3.0cm and the square glass of thickness 0.5mm, 2.3cm.In the Central Line of ito glass apart from two ends be 9mm position according to diameter be 1.5 ~ 2.0mm, thickness is that the mode of 6.0 ~ 10.0 μm is coated with above-mentioned liquid crystal sealing agent composition as bonding plane, is alignd in 1 limit of glass square with 2.3cm for ito glass square for 3.0cm and both are fitted, thus produce test film.After UV3000mJ is irradiated to the test film 10 of laminating, heat 60 minutes at 120 DEG C, liquid crystal sealing agent composition is solidified.(society of Shimadzu Seisakusho Ltd. manufactures to utilize Autograph; AGS) to solidification after test film ito glass Central Line on apart from end be that 5mm point carries out punching press, mensuration bonding strength.Its cohesive strength is 19.8N/mm.

Comparative example 1

Only containing component I, not containing component I I, all the other conditions are constant, and its cohesive strength is 12.3N/mm.

Comparative example 2

Only containing component I I, not containing component I, all the other conditions are constant, and its cohesive strength is 13.9N/mm.

Above-described embodiment and comparative example explanation, curing agent composition of the present invention, it is composite by two kinds of dissimilar solidifying agent, under same amount prerequisite, its cohesive strength will be better than far away being used alone of two kinds of components, proves to create synergistic effect between two kinds of solidifying agent that the present invention adopts.

Applicant states, the present invention illustrates curing agent composition of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned special formulation, does not namely mean that the present invention must rely on above-mentioned detailed component and formula could be implemented.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (2)

1. a curing agent composition, it comprises following component:

The mass ratio of two kinds of components described in described composition is 3:1-1:3.

2. curing agent composition as claimed in claim 1, it is characterized in that, the mass ratio of described two kinds of components is 2:1-1:2, preferred 2:1.