CN110157024B

CN110157024B - Pressure test membrane and preparation method thereof

Info

Publication number: CN110157024B
Application number: CN201810143406.3A
Authority: CN
Inventors: 崔叶; 董旭辉; 刘亚军; 李娜; 李亚想; 冉光念; 曹雪; 杨茉; 杨伟; 闫志鹏
Original assignee: Baoding Lucky Innovative Materials Co ltd
Current assignee: Aerospace Intelligent Manufacturing Technology Co ltd
Priority date: 2018-02-11
Filing date: 2018-02-11
Publication date: 2022-04-22
Anticipated expiration: 2038-02-11
Also published as: CN110157024A; WO2019154147A1

Abstract

The invention discloses a pressure test membrane and a preparation method thereof, the pressure test membrane comprises a bottom coating layer, a concave-convex structure layer, microcapsules and the like, wherein the concave-convex part of the concave-convex structure layer is provided with at least more than 2 convex parts, and the linear distance L between two adjacent convex parts meets the condition that D50x0.2 is more than or equal to L and is less than or equal to D50x 0.8.

Description

Pressure test membrane and preparation method thereof

Technical Field

The present disclosure relates to a concave-convex structure manufacturing apparatus, and more particularly, to a concave-convex structure manufacturing apparatus for manufacturing a concave-convex structure layer of a pressure test membrane.

Background

In each production process having a strict requirement on pressure, such as lamination of a printed circuit board, pressure confirmation and adjustment between rollers, attachment of a liquid crystal glass panel, assembly of an engine cylinder, and the like, a pressure test is often required.

To facilitate these pressure testing applications, pressure testing membranes have been used extensively. The pressure test membrane typically has a chromophoric portion and a chromogenic portion, the chromophoric portion comprising microcapsules containing electron-donating leuco dye precursors. The coloring portion is subjected to pressure to break the microcapsules therein to release the electron-donating leuco dye, and the electron-donating leuco dye contacts the electron-accepting compound to thereby color the coloring portion, and then the magnitude, the force point, and the like of the pressure are determined according to the coloring area, the chromaticity, and the like of the coloring portion.

In some types of chromophoric moieties, a relief structure layer, such as a spiked relief structure layer, is disposed between the chromonic layer (microcapsule layer) and a base coat layer supporting the chromonic layer to make microcapsules in a pressure test film more susceptible to rupture to release an electron-donating leuco dye and contact an electron-accepting compound to form color. Thus, even if a small pressure is applied to the pressure test membrane, high sensitivity of the pressure test membrane can be achieved.

In order to produce such a relief structure layer, a relief structure production apparatus is required.

Disclosure of Invention

The present disclosure has been made in view of the above-mentioned requirements. The present disclosure provides a device, which cooperates with the concave-convex structure material provided by the present disclosure, and can efficiently realize the preparation of the concave-convex structure through simple operation.

Specifically, according to an aspect of the present disclosure, there is provided a concave-convex structure layer manufacturing apparatus including: a conveying member for continuously feeding the undercoat layer sheet; a supply device in which a textured layer coating liquid is stored, the supply device being configured to apply the textured layer coating liquid on the undercoat layer sheet to form a coated textured structure wet-coated sheet having a uniform thickness; a forming device having a first relief structure on its own surface which is operatively conformed sufficiently to the coated relief structure wet coated sheet to form a second relief structure on the coated relief structure wet coated sheet surface opposite the first relief structure.

Preferably, the concavo-convex structure layer preparation device further comprises one or more pressing devices for helping the concavo-convex shape surface of the forming device to be sufficiently attached to the coated concavo-convex structure wet coating sheet.

Preferably, the pressing means is a press roller which rolls with the movement of the undercoat sheet.

Preferably, the forming means is a forming roller which rolls with the movement of the undercoat sheet.

Preferably, the concavo-convex structure layer preparing apparatus further includes an ultraviolet lamp which hardens the wet coating layer sheet having a specific concavo-convex shape to form a coated concavo-convex structure layer sheet.

Preferably, the concave-convex structure layer preparation equipment further comprises a sheet collecting device, and the sheet material with the concave-convex structure layer is collected for standby.

Preferably, the concavo-convex structure layer is formed of UV resin.

Preferably, the forming means are exchangeable, different forming means having different first relief structure shapes.

Preferably, the first relief structure of the forming device is adjustable in shape.

Preferably, the second concave-convex structure of the concave-convex structure layer has 2 or more convex portions, and the linear distance L between the top ends of the adjacent 2 convex portions satisfies the following relationship: D50X 0.2L 50X 0.8D 50 represents the corresponding particle size when the cumulative particle size distribution number of the microcapsules reaches 50%.

The concave-convex structure layer preparation equipment provided by the disclosure is simple, only three components can realize the formation of a concave-convex structure at least, and the sheets with the concave-convex structure layers meeting different requirements can be prepared by replacing the forming device and adjusting the shape of the concave-convex structure of the forming device.

Drawings

For a better understanding of the present disclosure and to describe more clearly how it may be carried into effect, the present disclosure will now be described, by way of example, with reference to the accompanying drawings, in which:

FIG. 1 is a schematic representation of the structure of a chromonic film material L according to one embodiment of the disclosure;

fig. 2 is a schematic view of a manufacturing apparatus of the concavo-convex structure layer shown in fig. 1 according to a first embodiment of the present disclosure; and

fig. 3 is a schematic view of a manufacturing apparatus of the concavo-convex structure layer shown in fig. 1 according to a second embodiment of the present disclosure.

Detailed Description

Reference will now be made in detail to specific embodiments for carrying out the present disclosure, with the understanding that the following description is to be construed as merely illustrative of certain preferred examples of the present disclosure and should not be construed as limiting the scope of the present disclosure. Other examples, features, aspects, embodiments, and advantages of the disclosure will become apparent to those skilled in the art from the following description. It should also be appreciated that any one or more of the concepts, expressions, embodiments, examples, etc. described in the disclosure may be combined with any one or more of the other concepts, expressions, embodiments, examples, etc. described in the disclosure. Therefore, the teachings, descriptions, embodiments, examples, etc. described below should not be considered independent of each other.

Additionally, the illustrations in the figures are not necessarily to scale, and in some instances, features of the disclosure may be exaggerated or minimized in the figures to facilitate an understanding of the disclosure. And in the drawings, like reference numerals generally refer to like features.

Fig. 1 is a schematic structural view of a color film according to one embodiment of the present disclosure. As shown in fig. 1, the color film is made of a color film material L composed of a color film base material 113, an undercoat layer 115, a relief structure layer 117, and a color layer 119. The undercoat layer 115, the relief structure layer 117, and the color development layer 119 are sequentially applied and attached to the color development film substrate 113. The structure and the function of the concavo-convex structure layer 117 will be described in more detail below.

Fig. 2 is a schematic view of a concave-convex structure layer production apparatus according to a first embodiment of the present disclosure. As shown in fig. 2, the concave-convex structure layer preparation apparatus according to the present embodiment includes a sheet-sending roller 210, a supply device 220, a conveying roller 230, a forming roller 240, an ultraviolet lamp 250, and a sheet-receiving roller 270.

In one embodiment according to the present disclosure, in the process of preparing the concave-convex structure layer 117 using the concave-convex structure layer preparing apparatus, a sheet is first continuously fed from the hairline roller 210 by the conveying roller 230. Here, the sheet is a material formed after the primer layer is coated on the substrate, that is, a composite sheet including the substrate 113 and the primer layer 115 shown in fig. 1.

The supply means 220 shown in FIG. 2 stores a coating liquid for a relief structure layer, and the composition and preparation process of the coating liquid will be described in detail later. During the operation of the concavo-convex structure layer preparing apparatus, the supply device 220 applies the coating liquid therein to the sheet passing therethrough to form a coated concavo-convex structure wet-coated sheet 280 having a uniform thickness.

The forming roller 240 has a special concavo-convex shape (pattern). As the textured wet coating sheet 280 passes over the forming roll 240, the concave-convex profile of the forming roll 240 conforms sufficiently to the textured wet coating sheet 280 to form a wet coating concave-convex shape on the textured wet coating sheet 280 opposite the concave-convex shape on the forming roll 240.

The ultraviolet lamp 250 is used to sufficiently irradiate the coated concavo-convex structure layer sheet 290, on which the wet coating concavo-convex shape has been formed, so that it is hardened to form the coated concavo-convex structure layer sheet 290 (i.e., a composite sheet including the substrate, the undercoat layer, and the concavo-convex structure layer shown in fig. 1).

The take-up roll 270 takes up the coated layer 290 for use. It is to be noted that the forming roll and the concavo-convex portions having a special concavo-convex shape or pattern on the concavo-convex structure layer will be described in more detail hereinafter.

Fig. 3 is a schematic view of a concave-convex structure layer production apparatus according to a second embodiment of the present disclosure. As shown in fig. 3, the concave-convex structure layer preparation apparatus in the present embodiment includes a sheet-sending roller 310, a supply device 320, a first pressing roller 330, a forming roller 340, an ultraviolet lamp 350, a second pressing roller 360, and a sheet-receiving roller 370. In the present embodiment, other components than the first pressing roller 330 and the second pressing roller 360 have similar functions to the same-named components in the first embodiment, and only different portions are described below.

In one embodiment according to the present disclosure, the present embodiment constitutes a transport section by the delivery roll 310 and the take-up roll 370 to continuously feed the substrate on which the undercoat layer is coated on the delivery roll.

The supply device 320 applies the concave-convex structure layer coating liquid stored therein to the substrate passing therethrough to form a coated concave-convex structure wet coating sheet 380 having a uniform thickness.

The first press roll 330 and the second press roll 360 cooperate with each other to sufficiently conform the concavo-convex shaped sheet 380 of the coated concavo-convex structure wet-coated sheet to the concavo-convex shaped curved surface of the forming roll 340 to form a concavo-convex shape on the concavo-convex shaped sheet 380 of the coated concavo-convex structure wet-coated sheet 380 that is opposed to the concavo-convex shaped curved surface of the forming roll 340.

As for the forming

rollers

240 and 340, they may have different concavo-convex shapes on their surfaces, and in the same concavo-convex structure layer preparing apparatus, the forming

rollers

240 and 340 are designed to be replaceable according to actual needs, so that one concavo-convex structure layer preparing apparatus can prepare

sheets

290 or 390 having various concavo-convex shapes.

In addition, the forming

rollers

240 and 340 may also be designed to manually or automatically adjust the concave-convex pattern thereon, such as adjusting the mutual distance between the respective convex or concave portions thereon, the height of the respective convex or concave portions, and the like.

< uneven Structure layer 117>

In one embodiment according to the present disclosure, the rugged structure layer 117 is used to apply the pressure applied to the surface of the pressure test membrane to the microcapsules in the color layer 119 after area conversion. The concavo-convex structure layer 117 is composed of a UV resin, a reactive diluent, and a photo initiator.

In one embodiment according to the present disclosure, the UV resin in the concavo-convex structure layer 117 is composed of two or more of the following UV resins, and the UV resin suitable for the present disclosure includes, but is not limited to, urethane acrylate, epoxy acrylate, aliphatic urethane acrylate, and the like. The reactive diluent in the concave-convex structure layer 117 is composed of two or more of the following reactive diluents, including but not limited to bifunctional monomers such as tripropylene glycol diacrylate (TPGDA), dipropylene glycol diacrylate (DPGDA), trifunctional monomers such as pentaerythritol triacrylate (PET3A), trimethylolpropane triacrylate (TMPTA), multifunctional monomers such as dipentaerythritol hexaacrylate (DPHA), pentaerythritol tetraacrylate (PET4A), and the like. Photoinitiators include, but are not limited to, 1-hydroxycyclohexyl phenyl ketone (184), 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide (TPO), 2-methyl-1- [ 4-methylthiophenyl ] -2-morpholino-1-propanone (907), and the like.

In one embodiment according to the present disclosure, the concavo-convex portion of the concavo-convex structure layer 117 has at least 2 or more convex portions, and a linear distance L between adjacent two convex portions satisfies D50X0.2 ≦ L ≦ D50X0.8. When L < D50X0.2, the distance between adjacent projections is too small, the microcapsule force-receiving area cannot be effectively concentrated, and pressure distribution measurement under a micropressure condition cannot be achieved, and when L > D50X0.8, most of the microcapsules are trapped in the spaces between adjacent projections, and the microcapsules cannot be broken to develop color when pressed, and pressure distribution measurement cannot be achieved.

In an embodiment according to the present disclosure, the convex shape of the concavo-convex structure layer 117 includes, but is not limited to, a cylindrical shape, a conical shape, a rectangular parallelepiped shape, a square cube shape, and the like.

Examples of various coating liquids (slurries)

Some components of the concave-convex structure layer coating liquid are given below, but the present disclosure is not limited thereto.

(example 1)

Preparation of undercoat slurry

6kg of styrene-butadiene copolymer latex (SBR)

10kg of polyvinyl alcohol PVA217 (10%)

84kg of water

6kg of SBR and 10kg of 10% PVA217 aqueous solution are added into 84kg of water, and after uniform stirring, a primer slurry is prepared for standby.

Preparation of coating liquid for concave-convex structure layer

Adding 20kg of epoxy acrylate into 40kg of polyurethane acrylate, uniformly stirring, sequentially adding 25kg of PET3A and 15kg of DPHA, uniformly stirring, adding 3kg of 184 and 3kg of TPO, and fully and uniformly stirring to obtain the concave-convex structure layer slurry for later use.

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

diisopropyl naphthalene 60kg

Crystal Violet Lactone (CVL) 3.0kg

2.4kg of colorless methylene blue (BLMB)

12kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

Adding 3.0kg of CVL and 2.4kg of BLMB into 60kg of diisopropylnaphthalene and 5kg of methyl ethyl ketone, stirring until the mixture is completely dissolved to obtain a dye solution for later use, adding 12kg of trimethylolpropane adduct of hexamethylene diisocyanate into the dye solution, and fully and uniformly stirring to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

40kg of 10% PVA217 aqueous solution is added into 60kg of water, and after uniform stirring, an aqueous phase solution is obtained for standby.

Aqueous solution of curing agent

Triethylene tetramine 5kg

20kg of water

And taking the water phase solution as a continuous mobile phase of a film emulsifier and the oil phase solution as a dispersion phase, obtaining microcapsule emulsion by adopting a film emulsification method, then adding a curing agent water solution into the obtained emulsion, heating to 50 ℃ under a stirring state, continuously reacting for 4 hours, cooling to room temperature, adding water to adjust the solid content to be 30%, and thus obtaining the microcapsule dispersion liquid containing the electron-donating leuco dye precursor.

Preparation of a chromonic layer dispersion

20kg of 10% PVA205 aqueous solution and 30kg of 10% CMC aqueous solution are sequentially added into 50kg of 30% microcapsule dispersion liquid, and after being uniformly stirred, 33kg of water is added to adjust the solid content to 15% to obtain the color development layer dispersion liquid for standby.

Preparation of color-developing layer dispersion

Adding 10kg of activated clay into 30kg of water, performing sand grinding dispersion by using a sand mill to obtain an activated clay water dispersion, adding 2kg of SBR and 2kg of gelatin, and uniformly stirring to obtain a color development layer dispersion for later use.

And (3) sequentially coating a 0.5-micrometer base coat layer and a concave-convex structure layer on a 75-micrometer polyethylene terephthalate (PET) base material by using a silk rod, coating a 12-micrometer color development layer by using a slide coater, drying and rolling to obtain the color development film material of the pressure test film.

A developing layer of 13 microns was coated on a 75 micron PET substrate using a wire rod to give the developing film material of the pressure test film described in this disclosure after drying and winding. The resulting chromophoric film material was tested for performance by overlaying it with a chromogenic film material in a coating-opposing manner.

(example 2)

Preparation of undercoat slurry

SBR 6kg

PVA217(10％) 10kg

84kg of water

Preparation of coating liquid for concave-convex structure layer

40kg of urethane acrylate

Epoxy acrylate 20kg

PET3A 22kg

DPHA 18kg

907 3kg

TPO 3kg

Adding 20kg of epoxy acrylate into 40kg of polyurethane acrylate, uniformly stirring, sequentially adding 22kg of PET3A and 18kg of DPHA, uniformly stirring, adding 3kg of 907 and 3kg of TPO, and fully and uniformly stirring to obtain the concave-convex structure layer slurry for later use.

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

diisopropyl naphthalene 60kg

CVL 4.4kg

BLMB 3.6kg

10kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

Adding 4.4kg of CVL and 3.6kg of BLMB into 60kg of diisopropylnaphthalene and 5kg of methyl ethyl ketone, stirring until the mixture is completely dissolved to obtain a dye solution for later use, adding 10kg of trimethylolpropane adduct of hexamethylene diisocyanate into the dye solution, and fully and uniformly stirring to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA205 aqueous solution (10%)

40kg of 10% PVA205 aqueous solution is added into 60kg of water, and after uniform stirring, an aqueous phase solution is obtained for standby.

Aqueous solution of curing agent

Ethylene diamine butylene oxide adduct 5kg

20kg of water

The microcapsule emulsion is obtained by using the water phase solution as the continuous mobile phase of the membrane emulsifier and the oil phase solution as the dispersed phase by adopting a membrane emulsification method. Then, an aqueous solution of a curing agent was added to the obtained emulsion, heated to 50 ℃ under stirring, and continuously reacted for 4 hours, followed by cooling to room temperature and adding water to adjust the solid content to 30%, thereby obtaining a microcapsule dispersion containing an electron-donating leuco dye precursor.

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

20kg of 10% PVA205 aqueous solution and 30kg of 10% CMC aqueous solution are sequentially added into 50kg of 30% microcapsule dispersion liquid, and after the uniform stirring, 33kg of water is added to adjust the solid content to 15% to obtain the color development layer dispersion liquid for standby.

Preparation of color-developing layer dispersion

Coating a 0.5-micrometer base coating layer on a 75-micrometer PET substrate by using a silk rod, coating a concave-convex structure layer according to the coating mode shown in the figure 3, coating a 12-micrometer color development layer by using a slide coater, drying and rolling to obtain the color development film material of the pressure test film.

(example 3)

Preparation of undercoat slurry

SBR 5kg

PVA117(10％) 15kg

80kg of water

5kg of SBR and 15kg of 10% PVA117 aqueous solution are added into 80kg of water, and after uniform stirring, primer slurry is prepared for standby.

Preparation of coating liquid for concave-convex structure layer

40kg of urethane acrylate

Epoxy acrylate 20kg

TPGDA 25kg

DPHA 15kg

184 3kg

TPO 3kg

Adding 20kg of epoxy acrylate into 40kg of polyurethane acrylate, uniformly stirring, sequentially adding 25kg of TPGDA and 15kg of DPHA, uniformly stirring, adding 3kg of 184 and 3kg of TPO, and fully and uniformly stirring to obtain the concave-convex structure layer slurry for later use.

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

60kg of 1-phenyl-1-dimethylphenylethane

CVL 1.5kg

BLMB 1.2kg

8kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

Adding 1.5kg of CVL and 1.2kg of BLMB into 60kg of 1-phenyl-1-dimethylphenylethane and 5kg of methyl ethyl ketone, stirring until the mixture is completely dissolved to obtain a dye solution for later use, adding 8kg of trimethylolpropane adduct of hexamethylene diisocyanate into the dye solution, and fully and uniformly stirring to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

Aqueous solution of curing agent

4kg of hexamethylenediamine

20kg of water

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

Preparation of color-developing layer dispersion

Coating a 0.5-micrometer base coat layer on a 75-micrometer PET substrate by using a silk rod, coating a concave-convex structure layer according to the coating mode shown in figure 3, coating a 12-micrometer color development layer by using a slide coater, drying and rolling to obtain the color development film material of the pressure test film.

(example 4)

Preparation of undercoat slurry

SBR 5kg

PVA217(10％) 15kg

80kg of water

5kg of SBR and 15kg of 10% PVA217 aqueous solution are added into 80kg of water, and after uniform stirring, primer slurry is prepared for standby.

Preparation of coating liquid for concave-convex structure layer

Urethane acrylate 35kg

Epoxy acrylate 25kg

PET3A 20kg

PET4A 20kg

184 3kg

907 3kg

Adding 25kg of epoxy acrylate into 35kg of polyurethane acrylate, uniformly stirring, sequentially adding 20kg of PET3A and 20kg of PET4A, uniformly stirring, adding 3kg of 184 and 3kg of 907, and fully and uniformly stirring to obtain the concave-convex structure layer slurry for later use.

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

diisopropyl naphthalene 60kg

CVL 3.0kg

BLMB 2.4kg

7.5kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

3.0kg of CVL and 2.4kg of BLMB are added into 60kg of diisopropylnaphthalene and 5kg of methyl ethyl ketone, stirred until the materials are completely dissolved to obtain a dye solution for later use, 7.5kg of trimethylolpropane adduct of hexamethylene diisocyanate is added into the dye solution, and the materials are fully stirred uniformly to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

Aqueous solution of curing agent

Triethylene tetramine 4kg

20kg of water

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

Preparation of color-developing layer dispersion

(example 5)

Preparation of undercoat slurry

SBR 6kg

PVA117(10％) 10kg

84kg of water

6kg of SBR and 10kg of 10% PVA117 aqueous solution were added to 84kg of water, and after stirring uniformly, a primer slurry was prepared for use.

Preparation of coating liquid for concave-convex structure layer

Adding 30kg of epoxy acrylate into 30kg of polyurethane acrylate, uniformly stirring, sequentially adding 30kg of DPGDA and 10kg of PET4A, uniformly stirring, adding 2.5kg of 184 and 4kg of TPO, and fully and uniformly stirring to obtain the concave-convex structure layer slurry for later use.

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

60kg of 1-phenyl-1-dimethylphenylethane

CVL 2.0kg

BLMB 1.6kg

12kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

2.0kg of CVL and 1.6kg of BLMB are added into 60kg of 1-phenyl-1-dimethylphenylethane and 5kg of methyl ethyl ketone, stirred until the mixture is completely dissolved to obtain a dye solution for later use, 12kg of trimethylolpropane adduct of hexamethylene diisocyanate is added into the dye solution, and the mixture is fully stirred uniformly to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

Aqueous solution of curing agent

Triethylene tetramine 5kg

20kg of water

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

Preparation of color-developing layer dispersion

30kg of water

Activated clay 10kg

SBR 2kg

Gelatin 2kg

Comparison with existing pressure test membranes

Comparative example 1

Preparation of undercoat slurry

SBR 6kg

PVA217(10％) 10kg

84kg of water

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

diisopropyl naphthalene 60kg

CVL 5.0kg

BLMB 3.8kg

12kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

Adding 5.0kg of CVL and 3.8kg of BLMB into 60kg of diisopropylnaphthalene and 5kg of methyl ethyl ketone, stirring until the mixture is completely dissolved to obtain a dye solution for later use, adding 12kg of trimethylolpropane adduct of hexamethylene diisocyanate into the dye solution, and fully and uniformly stirring to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

Aqueous solution of curing agent

Triethylene tetramine 5kg

20kg of water

And (3) adopting a mechanical emulsification method, taking the water phase solution as a continuous phase, adding the oil phase solution under the high-speed stirring state of 750rpm, and emulsifying for 10 minutes to obtain the microcapsule emulsion. Then, an aqueous curing agent solution was added to the obtained emulsion, heated to 50 ℃ with stirring, and after continuing the reaction for 4 hours, cooled to room temperature and added with water to adjust the solid content to 30%, thereby obtaining a microcapsule dispersion containing an electron donating leuco dye precursor.

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

Preparation of color-developing layer dispersion

30kg of water

Activated clay 10kg

SBR 2kg

Gelatin 2kg

And sequentially coating a 0.5-micrometer base coat on a 75-micrometer PET substrate by using a wire rod, coating a 12-micrometer color development layer by using a slide coater, drying and rolling to obtain the color development film material of the pressure test film.

A developing layer of 13 microns was coated on a 75 micron PET substrate using a wire rod, and dried and wound to give a developing film material of the pressure test film. The resulting chromogenic membrane material was overlayed with the chromogenic membrane material in a coating-opposing manner to test their performance.

Comparative example 2

Preparation of undercoat slurry

SBR 5kg

PVA217(10％) 15kg

80kg of water

Preparation of coating liquid for concave-convex structure layer

Production of microcapsules and dispersions thereof

Preparation of oil phase solution:

diisopropyl naphthalene 60kg

CVL 6.5kg

BLMB 5.4kg

12kg of trimethylolpropane adduct of hexamethylene diisocyanate

Methyl ethyl ketone 5kg

6.5kg CVL and 5.4kg BLMB are added into 60kg diisopropyl naphthalene and 5kg methyl ethyl ketone, stirred until the mixture is completely dissolved to obtain a dye solution for later use, 12kg trimethylolpropane adduct of hexamethylene diisocyanate is added into the dye solution, and the mixture is fully stirred uniformly to obtain an oil phase solution for later use.

Preparation of aqueous phase solution:

60kg of water

40kg of PVA217 aqueous solution (10%)

Aqueous solution of curing agent

Triethylene tetramine 5kg

20kg of water

And (3) adopting a mechanical emulsification method, taking the water phase solution as a continuous phase, adding the oil phase solution under the high-speed stirring state of 950rpm, and emulsifying for 10 minutes to obtain the microcapsule emulsion. Then, an aqueous curing agent solution was added to the obtained emulsion, heated to 50 ℃ with stirring, and after continuing the reaction for 4 hours, cooled to room temperature and added with water to adjust the solid content to 30%, thereby obtaining a microcapsule dispersion containing an electron donating leuco dye precursor.

Preparation of a chromonic layer dispersion

50kg of microcapsule Dispersion (30%)

20kg of PVA205 aqueous solution (10%)

30kg of CMC water solution (10 percent)

33kg of water

A 0.5-micron primer layer was sequentially coated on a 75-micron PET substrate using a wire rod, a relief structure layer was coated according to the coating method shown in fig. 3, a 12-micron color layer was coated using a slide coater, dried, and wound to obtain a color-developing film material of a pressure test film.

TABLE 1 Performance test data sheet for each example

D50/μm

span

A/μm

Applicability to Low temperature color development

Sensitivity of the test

Apparent uniformity

Example 1

8.3

0.71

5.8

A

Example 2

10.7

1.02

7.5

A

Example 3

6.1

0.62

4.4

A

Example 4

8.9

0.75

5.8

A

Example 5

7.4

0.72

3.7

A

Comparative example 1

16.4

1.53

/

B

C

Comparative example 2

8.5

1.21

5.8

C

B

In the table, the test methods for the respective properties are as follows:

1. method for testing particle size distribution

And (3) taking the microcapsule dispersion, and testing by using a BT-9300ST type laser particle size distribution instrument to obtain the particle size distribution D50 and the particle size distribution span of the microcapsule dispersion.

Method for testing A value

The shortest distance between 5 sets of adjacent protrusions was measured under an electron microscope (SEM) from a sheet coated with the undercoat layer and the relief structure layer, and the average value was obtained to obtain the a value.

3. Method for testing low-temperature color development applicability

The pressure test membranes obtained above were divided into two groups I and II, and the following tests were carried out at 25 ℃ and 10 ℃ respectively. The microcapsules are first cut into 3cmX3cm size, then the color development sheet containing electron-donating leuco dye precursor and the color development sheet containing electron-accepting compound are overlapped in a manner that the coatings are opposite, and placed between two smooth planes, the whole sheet is pressed to be fully covered to make the sheet saturated and develop color, then the overlapped two sheets are peeled off, the concentration value OD1 of the color development part on the color development sheet is measured by an X.rite colorimeter, the initial concentration value OD0 of the non-color development part of the color development sheet is measured by the same method, and the actual color development concentration OD is obtained by OD1-OD 0. The difference delta OD of the color development concentration of the two groups of sheets under the same pressure at different temperatures can be obtained by using OD I-OD II.

Evaluation criteria

A (1.5. ltoreq. OD,. DELTA.OD. ltoreq.0.2): the dye is not separated out at 10 ℃ and can be normally used;

b (1.3 < OD <1.5, 0.2< Δ OD < 0.4): the dye is slightly separated out at 10 ℃, and the use is not influenced;

c (OD <1.3,. DELTA.OD > 0.4): the dye is seriously separated out at 10 ℃ and cannot be normally used;

4. test sensitivity test method

The pressure test film obtained above was cut into a size of 20cmX20cm, and then a color development sheet containing an electron donating leuco dye precursor and a color development sheet containing an electron accepting compound were overlapped with the coatings facing each other and placed between two smooth planes, and the entire sheet was subjected to full-coverage pressure to develop color, after which the overlapped two sheets were peeled off, and color development concentration values ODi of 5 groups of different regions were randomly measured on the color development sheet by an x.rite colorimeter to obtain an average value OD, and a maximum error value Δ OD was obtained, and the percentage value X was obtained by dividing the Δ OD by the Δ OD.

A (X is less than or equal to 5%): the boundary is clear and identifiable, and the test sensitivity is high;

b (5% < X ≦ 10%): the definition of the boundary can be accepted, and the test sensitivity can be accepted;

c (10% < X): the boundary is fuzzy, and the test sensitivity is poor;

5. apparent uniformity testing method

The pressure test film obtained above was cut into a size of 10cmX10cm, 5 areas were randomly selected, and the appearance of the microcapsules was observed by an electron microscope.

A, uniformly spreading large and small particles without agglomeration;

b, the large and small particles are spread basically and uniformly without obvious agglomeration;

c, the small particles are not spread uniformly, and the small particles are close to the large particles to form an island-shaped structure;

as can be seen from the test results in the table, the low-temperature color development applicability, the test sensitivity and the apparent uniformity are all superior to those of the comparative example, so that the pressure test membrane prepared by adopting the technical scheme disclosed by the invention can meet the use requirement of a low-temperature environment, and can realize high-sensitivity and high-resolution pressure distribution test.

The present disclosure is not limited to the embodiments shown in the drawings and described in the specification. The foregoing description is illustrative only and is not limiting of the scope of the disclosure. Many variations are possible which remain within the concept and scope of the disclosure, as will be apparent from the above description.

Claims

1. A preparation method of a pressure test membrane comprises the steps of preparing a primer slurry, preparing a concave-convex structure layer coating liquid, preparing microcapsules and dispersion liquid thereof, preparing a color development layer dispersion liquid, and is characterized in that:

the preparation of the base coat slurry comprises the following steps:

selecting: styrene-butadiene copolymer latex SBR, having a mass of 6 kg; 10% polyvinyl alcohol PVA217 with a mass of 10 kg; 84kg of water; adding 6kg of SBR and 10kg of 10% PVA217 aqueous solution into 84kg of water, and uniformly stirring to prepare primer slurry;

the preparation of the concave-convex structure layer coating liquid comprises the following contents:

selecting:

adding 20kg of epoxy acrylate into 40kg of polyurethane acrylate, uniformly stirring, sequentially adding 25kg of PET3A and 15kg of DPHA, uniformly stirring, adding 3kg of 184 and 3kg of TPO, and fully and uniformly stirring to obtain concave-convex structure layer slurry;

the preparation of the microcapsule and the dispersion liquid thereof comprises the following steps: preparing oil phase solution, preparing water phase solution, preparing curing agent water solution,

the preparation of the oil phase solution comprises the following steps:

selecting: diisopropyl naphthalene with a mass of 60 kg; crystal violet lactone CVL with a mass of 3.0 kg; colorless methylene blue BLMB, the mass of which is 2.4 kg; a trimethylolpropane adduct of hexamethylene diisocyanate having a mass of 12 kg; methyl ethyl ketone, the mass of which is 5 kg;

adding 3.0kg of CVL and 2.4kg of BLMB into 60kg of diisopropylnaphthalene and 5kg of methyl ethyl ketone, stirring until the materials are completely dissolved to obtain a dye solution for later use, adding 12kg of trimethylolpropane adduct of hexamethylene diisocyanate into the dye solution, and fully and uniformly stirring to obtain an oil phase solution;

the preparation of the aqueous phase solution comprises the following steps:

selecting: water, the mass of which is 60 kg; a 10% aqueous PVA217 solution having a mass of 40 kg;

adding 40kg of 10% PVA217 aqueous solution into 60kg of water, and uniformly stirring to obtain an aqueous phase solution;

the preparation of the curing agent aqueous solution comprises the following steps:

selecting: triethylene tetramine, the mass of which is 5 kg; water, the mass of which is 20 kg;

taking the water phase solution as a continuous mobile phase of a film emulsifier and the oil phase solution as a dispersion phase, obtaining microcapsule emulsion by adopting a film emulsification method, then adding a curing agent aqueous solution into the obtained emulsion, heating to 50 ℃ under a stirring state, continuously reacting for 4 hours, cooling to room temperature, adding water to adjust the solid content to be 30%, and thus obtaining microcapsule dispersion liquid containing the electron-donating leuco dye precursor;

the preparation of the chromonic layer dispersion comprises the following steps:

selecting:

sequentially adding 20kg of 10% PVA205 aqueous solution and 30kg of 10% CMC aqueous solution into 50kg of 30% microcapsule dispersion liquid, uniformly stirring, and adding 33kg of water to adjust the solid content to 15% to obtain a color development layer dispersion liquid;

the preparation of the color development layer dispersion liquid comprises the following contents:

selecting:

adding 10kg of activated clay into 30kg of water, performing sand grinding dispersion by using a sand mill to obtain an activated clay water dispersion, adding 2kg of SBR and 2kg of gelatin, and uniformly stirring to obtain a color development layer dispersion;

sequentially coating a 0.5-micrometer base coat and a concave-convex structure layer on a 75-micrometer polyethylene terephthalate (PET) base material by using a silk rod, coating a 12-micrometer color development layer by using a slide coater, drying and rolling to obtain a color development film material of the pressure test film;

coating a 13-micron color development layer on a 75-micron PET (polyethylene terephthalate) base material by using a silk rod, drying and rolling to obtain a color development film material of the pressure test film, and overlapping the obtained color development film material and the color development film material in a coating opposite mode to obtain the pressure test film;

the concave-convex part of the concave-convex structure layer is provided with at least more than 2 convex parts, and the linear distance L between two adjacent convex parts meets the condition that D50x0.2 is more than or equal to L is more than or equal to D50x 0.8.

2.A pressure test membrane produced by the method for producing a pressure test membrane according to claim 1.