阅读说明：本技术 一种快速检验热固化胶粘剂脱泡效果的方法 (A kind of method of quick inspection hot setting adhesive deaeration effect ) 是由 桑广艺 夏佳斌 钱立飞 陶小乐 何永富 于 2019-10-12 设计创作，主要内容包括：本发明提供了一种快速检验热固化胶粘剂脱泡效果的方法,通过测试固化后的热固化胶粘剂的比重判断所述热固化胶粘剂的脱泡效果。将所述测试试样的比重与所述合格试样的比重进行比较,当所述测试试样的比重小于所述合格试样的比重时,则待测热固化胶粘剂的脱泡效果不合格；当所述测试试样的比重在所述合格试样的比重范围内时,则待测热固化胶粘剂的脱泡效果合格。该方法简单,便捷,可以用于对胶产品的脱泡效果进行评估。(The present invention provides a kind of methods for quickly examining hot setting adhesive deaeration effect, and the specific gravity by testing the hot setting adhesive after solidifying judges the deaeration effect of the hot setting adhesive.The specific gravity of the test sample is compared with the specific gravity of the qualified sample, when the specific gravity of the test sample is less than the specific gravity of the qualified sample, then the deaeration effect of hot setting adhesive to be measured is unqualified；When the specific gravity of the test sample is in the specific gravity range of the qualified sample, then the deaeration effect of hot setting adhesive to be measured is qualified.This method is simple, convenient, can be used for assessing the deaeration effect of glue product.)

1. a kind of method for quickly examining hot setting adhesive deaeration effect, which is characterized in that by testing the thermosetting after solidifying The specific gravity for changing adhesive judges the deaeration effect of the hot setting adhesive.

2. the method according to claim 1, wherein the following steps are included:

A) hot setting adhesive to be measured is filled into mold and is sufficiently solidified, after demoulding, obtains test sample, described in measurement The specific gravity of test sample；

B the specific gravity of the test sample is compared with the specific gravity of qualified sample), judges the deaeration of hot setting adhesive to be measured Effect.

3. according to the method described in claim 2, it is characterized in that, step B) are as follows: by the specific gravity of the test sample with it is described The specific gravity of qualified sample is compared, when the specific gravity of the test sample is less than the specific gravity of the qualified sample, then to calorimetric The deaeration effect of cured adhesive is unqualified；When the specific gravity of the test sample is in the specific gravity range of the qualified sample, Then the deaeration effect of hot setting adhesive to be measured is qualified.

4. the method according to claim 1, wherein the hot setting adhesive is selected from single-component thermosetting epoxy Adhesive.

5. the method according to claim 1, wherein the hot setting adhesive prepare in raw material do not include by Heat release gas generates bubble or the heated rear substance that volume expansion can occur itself.

6. the method according to claim 1, wherein stomata is closing in hot setting adhesive after the solidification Formula stomata.

7. according to the method described in claim 2, it is characterized in that, step A) in, the mold is heatproof mold.

Technical field

The invention belongs to adhesive technology fields, and in particular to a kind of side for quickly examining hot setting adhesive deaeration effect Method.

Background technique

In adhesive, the exploitation of sealant and manufacturing link, how to judge that deaeration effect is always a process difficulties. The quality of deaeration quality directly affects the final performance of glue product.The source of bubble is complicated, some are dissolved in liquid material Or gaseous matter, some air being introduced from outside into from mechanical mass dispersion process (such as stirring) contained；Also it comes from Gas medium in solid powder in particulate interspaces.It is unpractical for absolutely eliminating bubble.Common defoaming technology method is true (high speed) dispersion deaeration and (or) addition defoaming agent defoaming under empty condition.These means can effectively eliminate visible bubble, But it is helpless for superfine small bubble.It can not detect by an unaided eye.

Industry is not passed through at present, the method that intuitive or easy mode directly evaluates deaeration effect. In general the method that can be observed by the naked eye for the glue of pellucidity (the 1st class situation).But it is limited to the resolution energy of naked eye Power is helpless for extremely tiny such as tens microns of this methods of bubble below；2nd class situation, for containing Solid packing component is in appearance the adhesive or sealant of paste dope, is that can not or be difficult to carry out science by naked eyes It judges；Observation glue surface situation can be smeared by scraper to be evaluated, but often unreliable；In this case, feasible to do Method is to infer the quality of deaeration effect indirectly by the detection to glue properties of product.These performances are necessarily with air bubble content It is how many closely related, for example for structure glue, bubble can mostly reduce the mechanical strength of glue, this is needed by professional equipment, For example Material Testing Machine does mechanical test, however judgment method time-consuming consumes object.Therefore the inspection of a quick and easy operation is established The method for testing detection deaeration effect is most important.

Summary of the invention

In view of this, the technical problem to be solved in the present invention is that providing a kind of quickly inspection hot setting adhesive deaeration effect The method of fruit, the present invention judge that the deaeration of the hot setting adhesive is imitated by testing the specific gravity of the hot setting adhesive after solidifying Fruit, method are quick and easy.

The present invention provides a kind of methods for quickly examining hot setting adhesive deaeration effect, by testing the heat after solidifying The specific gravity of cured adhesive judges the deaeration effect of the hot setting adhesive.

Preferably, comprising the following steps:

A) hot setting adhesive to be measured is filled into mold and is sufficiently solidified, after demoulding, obtains test sample, is measured The specific gravity of the test sample；

B the specific gravity of the test sample is compared with the specific gravity of qualified sample), judges hot setting adhesive to be measured Deaeration effect.

Preferably, step B) are as follows: the specific gravity of the test sample is compared with the specific gravity of the qualified sample, works as institute When stating the specific gravity of test sample and being less than the specific gravity of the qualified sample, then the deaeration effect of hot setting adhesive to be measured is unqualified； When the specific gravity of the test sample is in the specific gravity range of the qualified sample, then the deaeration effect of hot setting adhesive to be measured It is qualified.

Preferably, the hot setting adhesive is selected from single-component thermosetting epoxy adhesive.

Preferably, preparing in raw material for the hot setting adhesive does not include after heated release gas generates bubble or is heated The substance of volume expansion itself can occur.

Preferably, stomata is enclosed type in the hot setting adhesive after the solidification.

Preferably, step A) in, the mold is heatproof mold.

Compared with prior art, the present invention provides a kind of method for quickly examining hot setting adhesive deaeration effect, lead to The specific gravity for crossing the hot setting adhesive after test solidifies judges the deaeration effect of the hot setting adhesive.By the test sample Specific gravity be compared with the specific gravity of the qualified sample, when the specific gravity of the test sample is less than the specific gravity of the qualified sample When, then the deaeration effect of hot setting adhesive to be measured is unqualified；When the test sample specific gravity the qualified sample ratio When in weight range, then the deaeration effect of hot setting adhesive to be measured is qualified.This method is simple, convenient, can be used for glue product Deaeration effect assessed.

Detailed description of the invention

Fig. 1 is the photo of product section prepared by embodiment 1 and embodiment 2；

Fig. 2 is the photo of product section prepared by embodiment 3 and embodiment 4.

Specific embodiment

The present invention provides a kind of methods for quickly examining hot setting adhesive deaeration effect, by testing the heat after solidifying The specific gravity of cured adhesive judges the deaeration effect of the hot setting adhesive.

Method provided by the invention is selected from single-component thermosetting mainly for hot setting adhesive, the hot setting adhesive Epoxy adhesive.

Preparing in raw material for the hot setting adhesive does not include that heated release gas generates bubble or heated rear meeting itself The substance of volume expansion occurs.Wherein, the substance of the heated release gas generation bubble and rear itself can occur that be heated Substance that the substance of volume expansion is known to the skilled person, such as azo-compound, expandable microspheres etc..

The component of volume expansion, such as azo compound can occur for itself containing in cured condition in formula, Expandable microspheres etc., the method are simultaneously not suitable for.Because volume expansion caused by these components is heated swollen compared to the bubble that glue itself contains Swollen volume change degree may be much larger.

Specific gravity by testing the hot setting adhesive after solidifying judges the deaeration effect of the hot setting adhesive.It is described Stomata is enclosed type in hot setting adhesive after solidification.For the gluing for generating a large amount of continuous open-celled structures internal after solidifying Agent, this law is simultaneously not suitable for, because open-celled structure directly affects the accuracy of specific gravity data.

Specifically, rapid detection method provided by the invention the following steps are included:

A) hot setting adhesive to be measured is filled into mold and is sufficiently solidified, after demoulding, obtains test sample, is measured The specific gravity of the test sample；

B the specific gravity of the test sample is compared with the specific gravity of qualified sample), judges hot setting adhesive to be measured Deaeration effect.

The present invention, which fills hot setting adhesive to be measured into mold, sufficiently to be solidified, and after demoulding, obtains test sample, Measure the specific gravity of the test sample.

Wherein, there is no specifically limited, art technologies by preparation process of the present invention to the hot setting adhesive to be measured Method well known to personnel.

The hot setting adhesive to be measured is filled into mold, wherein the mold is heatproof mold.The filling Method is that hot setting adhesive to be tested is filled into mold by casting mode or blade coating mode.Then, it is solid to treat calorimetric Change adhesive and carry out heat cure, wherein the present invention to the process conditions of the heat cure there is no specifically limited, according to adhesive Type is different, and the process conditions of the adjustment heat cure of adaptability guarantee that adhesive sufficiently solidifies.

It is demoulded after adhesive cooling after sufficiently solidifying, obtains test sample.Wherein, the method for the cooling is Natural cooling is cooled to room temperature condition.Wherein, the room temperature is defined as 25 ± 5 DEG C by the present invention.

Then the specific gravity of the test sample is measured, there is no specifically limited, abilities for method of the present invention to test specific gravity Specific weight determine method well known to field technique personnel.

The specific gravity of obtained test sample is compared with the specific gravity of qualified sample.Wherein, the ratio of the qualified sample The test method and process conditions of weight are identical as test method to be tested and process conditions.

Wherein, the qualified sample, which fills the hot setting adhesive of deaeration qualification into mold, is sufficiently solidified, and is taken off It is obtained after mould.Mould therefor and fill method, curing method and release method are all identical as sample to be tested, do not do herein superfluous It states.

The deaeration qualification refers to that parameter selection is reasonable in adhesive-preparing technology condition relative maturity, and colloidality, which can reach to apply, to be needed The state for asking requirement, specifically may include in have: speed of agitator meet dispersion require, jitter time long enough, vacuum degree foot The attainable best dispersity of glue in the case where enough high, at this time it is considered that bubble present in glue have reached homeostasis or Do not influence normal use.The specific gravity values measured at this time are in a reasonable section.

The specific gravity that the present invention is measured using the adhesive of deaeration qualification is measurement standard, by the specific gravity of the test sample and institute The specific gravity for stating qualified sample is compared, when the specific gravity of the test sample is less than the specific gravity of the qualified sample, then to be measured The deaeration effect of hot setting adhesive is unqualified；When the specific gravity of the test sample is in the specific gravity range of the qualified sample When, then the deaeration effect of hot setting adhesive to be measured is qualified.

Method provided by the invention is simple, convenient, can be used for assessing the deaeration effect of glue product.

For a further understanding of the present invention, below with reference to embodiment to quick inspection hot setting adhesive provided by the invention The method of deaeration effect is illustrated, and protection scope of the present invention is not limited by the following examples.

The equipment that following embodiment uses:

Planet dispersion machine: Wuxi Xu Ke robot Co., Ltd KXD series -5L；

High speed disperser: Flack Tek company, SpeedMixer DACC400.2 Germany.

Structure glue formula is shown in Table 1

Table 1

Raw material title	Mass parts	The trade mark	Supplier
				Liquid epoxies	100	BE188-90	Changchun chemical industry (Jiangsu) Co., Ltd
Liquid core shell rubbers	60	MX154	Kaneka (Japan)
				Acrylonitrile butadiene rubber modified epoxy resin	30	CTBN-861340	Shenzhen Jia Dida Chemical Co., Ltd.
Dicy-curing agent	6	Dyhard 100S	AlzChem A Ziken (Shanghai) Chemical Co., Ltd.
				Curing accelerator	2	UR300	AlzChem A Ziken (Shanghai) Chemical Co., Ltd.
Thickener	2	R202	Ying Chuan Specialty Chemical (Shanghai) Co., Ltd.
				Water absorbing agent	0.5	CaO	Shanghai Fan Hua inorganic chemical industry Co., Ltd
Pearl filler	50	S-CCR-100	Jiande Shuangchao Calcium Industry Co., Ltd.
				Pigment	0.2	057-4O3593	BOMEX Bao Meishi chemical color company

Conductive silver glue formula, is shown in Table 2

Table 2

Raw material title	Mass parts	The trade mark	Supplier
				O-cresol formaldehyde epoxy resin	40	SQCN700-1	Jinan holy well group
Bisphenol F-epoxy resin	20	NPEF-170	Changchun epoxy
				Diluent	24	1,4- butanediol diglycidyl ether	Nantong Hao Jin Chemical Co., Ltd.
Amine hardener	10	4,4- diaminodiphenylsulfone	Zhejiang Province Ding-long Chemical Co., Ltd
				Ureas promotor	5	Dyhard UR300	AlzChem A Ziken (Shanghai) Chemical Co., Ltd.
Silane coupling agent	1	Z6040	Dow corning company
				Conductive silver powder	300	Silver Flake EA-0290	Metalor company, the U.S.