CN109374165A - A kind of pressure detecting paper and preparation method thereof - Google Patents

A kind of pressure detecting paper and preparation method thereof Download PDF

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Publication number
CN109374165A
CN109374165A CN201811172937.1A CN201811172937A CN109374165A CN 109374165 A CN109374165 A CN 109374165A CN 201811172937 A CN201811172937 A CN 201811172937A CN 109374165 A CN109374165 A CN 109374165A
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parts
pressure
color
pressure detecting
agent
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CN109374165B (en
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张光明
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DONGGUAN ASTEED ELECTRONIC Co Ltd
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DONGGUAN ASTEED ELECTRONIC Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/24Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet
    • G01L1/247Measuring force or stress, in general by measuring variations of optical properties of material when it is stressed, e.g. by photoelastic stress analysis using infrared, visible light, ultraviolet using distributed sensing elements, e.g. microcapsules

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  • General Physics & Mathematics (AREA)
  • Color Printing (AREA)

Abstract

The present invention relates to field of display technology, more particularly to a kind of pressure detecting paper and preparation method thereof, including paper layer and it is adhered to the pressure-sensitive color layer of paper layer, the pressure-sensitive color layer is made by the raw material of following weight point: 15-30 parts of leuco dye microcapsules, 9-18 parts of interval dose, 10-15 parts of adhesive, 15-30 parts of color developer microcapsule, 1-3 parts of surfactant and 30-45 parts of solvent.The paper of the pressure detecting paper is smooth, any surface finish, and the pressure-sensitive color layer coated on paper layer is not easy to lose powder, stain resistant, color inhibition, and the density that develops the color and color development speed are preferable.

Description

A kind of pressure detecting paper and preparation method thereof
Technical field
The present invention relates to field of display technology, and in particular to a kind of pressure detecting paper and preparation method thereof.
Background technique
In process of production, need to be monitored the pressure condition of equipment, it is main at present using pressure measurement film come Pressure, pressure distribution and pressure balance of measuring device etc..
Currently used pressure measurement film is divided into monolithic type and Double-piece type, wherein monolithic type pressure-sensitive paper is on substrate It is coated with substance that show color, substance that show color upper layer is equipped with microcapsule layer again, color-producing bodies, working principle are enclosed in microcapsules Be: when pressure, chemistry occurs for microcapsules rupture instead with the substance that show color on film after the interior color-producing bodies outflow wrapped up of microcapsules It answers, occurs color area on film, and color density changes with the change of stress level.
But existing microcapsules are easy to damage in use, and microcapsules is caused to rupture too early, package in microcapsules Volume color-producing bodies and substance that show color haptoreaction, pressure measurement film develops the color in advance leads to scrap of the product;In addition, existing colour developing Substance is coated on substrate, is exposed to the atmosphere easily is oxidized jaundice for a long time.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of pressure detectings Paper, paper is smooth, any surface finish, and the pressure-sensitive color layer coated on paper layer is not easy to lose powder, stain resistant, color inhibition, and develop the color density It is preferable with color development speed.
Another object of the present invention is to provide a kind of preparation methods of pressure detecting paper, and the preparation method is easy to operate, Easy to control, high production efficiency, production cost is low, can be used for being mass produced.
The purpose of the invention is achieved by the following technical solution: a kind of pressure detecting paper, including paper layer and is adhered to paper The pressure-sensitive color layer of layer, the pressure-sensitive color layer are made by the raw material of following weight point:
Pressure detecting paper of the invention, paper is smooth, any surface finish, and the pressure-sensitive color layer coated on paper layer is not easy to lose powder, Stain resistant, color inhibition, the density that develops the color and color development speed are preferable.Using the color developing agent coating of the color developer microcapsule substitution prior art In paper layer, the anti-yellowing property of color developing agent is improved, and color developer microcapsule plays the role of compensator or trimmer pressure, reduces interval dose The collective effect of usage amount, color developer microcapsule and interval dose improves the compressive property of pressure detecting paper, avoids pressure detecting paper It damages in use, premature colouration causes paper to be scrapped;The surfactant of addition improves the wetability of pressure-sensitive color layer Can, it reduces the surface tension of pressure-sensitive color layer and improves the flatness of pressure-sensitive color layer, slow down because of color developer microcapsule and interval The use of agent causes smoothness to lower, and improves the quality of pressure detecting paper;The adhesive of addition keeps pressure-sensitive color layer and paper layer viscous One is invested, if addition adhesive is excessive, is easy to make paper warpage, dosage is very little, is easy to make leuco dye microcapsules, color developing agent Microcapsules and interval dose fall off, and reduce the colour developing density of pressure detecting paper.
Preferably, the partial size of the leuco dye microcapsules be 0.2-4 μm, the leuco dye microcapsules, interval dose and The partial size ratio of color developer microcapsule is 1:3-5:2-3.
Through the above technical solutions, it is micro- to avoid leuco dye under the double protection of interval dose and color developer microcapsule Capsule is ruptured in transport, use process by external force;The size controlling of leuco dye microcapsules, can be with interval at 0.2-4 μm Agent and color developer microcapsule clearance fit improve the flatness of pressure-sensitive color layer, lower fluffing rate, improve pressure-resistant performance;If hidden The partial size of color dye microcapsule is greater than 4 μm, and cyst wall pressure resistance degradation, leuco dye microcapsules hold in transport, coating process It is easily rupturable, the quality of product is reduced, when the partial size of leuco dye microcapsules is less than 0.2 μm, pressure-resistant performance is improved, but is needed The wall material of consumption increases, and improves production cost, the size controllings of leuco dye microcapsules at 0.2-4 μm, partial size it is of different sizes, Voltage endurance capability is also different, and it is easily different to apply the different colour developing density of pressure to pressure detecting paper;If the partial size of interval dose is excessive, It is settled before coating pressure-sensitive color layer, so that coating is uneven, colour developing density is caused to lower, colour developing is interrupted, and works as interval dose Partial size it is too small, can not play the role of protect leuco dye microcapsules;If the partial size of color developer microcapsule is excessive, resistance to pressure energy Power is weak, is easy to damage in transport, use process, if the partial size of color developer microcapsule is too small, can not play protection leuco dye The effect of microcapsules, and the colour developing agent content in color developer microcapsule is few, colour developing density is low, and color developing effect is poor.
Preferably, the interval dose is at least one of starch, silica sand, casein, kaolin and calcium carbonate;The glue Stick is at least one of styrene-butadiene latex, carboxylic styrene butadiene latex, propyl benzene latex and modified starch.
The interval dose of addition can prevent leuco dye microcapsules and color developer microcapsule in transport, use process by outer Power rupture not only can prevent leuco dye microcapsules and color developer microcapsule from existing it is furthermore preferred that the interval dose is calcium carbonate It is ruptured in transport, use process by external force, also substantially improves the thixotropy of system, be remarkably improved the attachment of pressure-sensitive color layer Power, stain resistance improve intensity and surface smoothness, and have good anti-settling effect, avoid influencing pressure detecting paper Develop the color density.The adhesive of addition makes pressure-sensitive color layer and paper layer be adhered to one, it is furthermore preferred that the adhesive is carboxyl fourth With weight ratio 1:2 mixing, the synergistic effect of carboxylic styrene butadiene latex and modified starch improves adhesive for benzene latex and modified starch Adhesive property;The modified starch is oxidized starch or cationic starch, helps to improve the retention of interval dose, improves product Quality.
Preferably, the surfactant is at least one in sodium alginate, sodium carboxymethylcellulose and methylcellulose Kind;The solvent is water or ethyl alcohol.
The wettability of pressure-sensitive color layer can be improved in the surfactant of addition, reduce pressure-sensitive color layer surface tension and The flatness for improving pressure-sensitive color layer slows down because the use of color developer microcapsule and interval dose causes smoothness to lower, improves pressure The quality of power detection paper;It is furthermore preferred that the surfactant is that sodium carboxymethylcellulose and methylcellulose are with weight ratio 3-5:1 mixing, further increases the wettability of pressure-sensitive color layer, reduces the surface tension of pressure-sensitive color layer and improves pressure-sensitive aobvious The flatness of chromatograph.The solvent is water or ethyl alcohol, reduces cost of material.
Preferably, the preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) weighing 1-4 parts of leuco dyes, 35-45 parts of solvent naphthas, 40-50 parts of mass fractions by weight is 4-8%'s Esterification modification SMA- aqueous solution, 25-35 parts of melamines, 10-25 parts of formaldehyde and 10-15 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 50-60 DEG C, obtain dye solution;In 900- Under 1300rpm revolving speed, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 1800-2200rpm, emulsification point 1-2h is dissipated, emulsified solution A is obtained, it is spare;
(A3) it takes melamine and formaldehyde to be uniformly mixed, alkaline conditioner is added and adjusts pH value to 8-8.5, at 50-80 DEG C At a temperature of, 1-2h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator It is acidified 0.8-1.2h, pH value is adjusted to 6-6.5, is warming up to 58-60 DEG C, continues to be acidified 0.3-0.6h, adjust pH value to 5.0- 5.5,1.5-2h is kept the temperature, then adjust pH value to 4-4.5, keeps the temperature 1.5-2h, stand 7-9h, leuco dye microcapsules are made in filtering.
Using leuco dye microcapsules made from above-mentioned preparation method, particle diameter distribution is existing without being mutually adhered at 0.2-4 μm As, and good airproof performance, ball-type are complete.Wherein, in step (A2), stirring promotes leuco dye to be dissolved in molten at 50-60 DEG C In agent oil, production efficiency is improved, under 900-1300rpm revolving speed, dye solution is dispersed in esterification modification SMA- aqueous solution, Under 1800-2200rpm revolving speed, reaching homo-effect, the droplet distribution of formation is at 2-4 μm, if revolving speed is too low, size droplet diameter Bigger than normal and particle size distribution range is wider, if revolving speed is too high, is easy blistering, is unfavorable for microcapsules molding;Use mass fraction for 4- 8% esterification modification SMA- aqueous solution facilitates dye solution and disperses to be formed that partial size is smaller, partial size in water phase as emulsifier The drop of narrow distribution, moreover it is possible to adsorb prepolymer and be enriched with to the droplet surface of dispersion.In step (A3), adjusted with alkaline conditioner PH value promotes melamine and formaldehyde that condensation reaction occurs, forms prepolymer A to 8-8.5.In step (A4), emulsified solution A with Prepolymer A mixing, under the effect of esterification modification SMA- aqueous solution, the surface enrichment prepolymer A of emulsified solution A, in acidization In, acid regulator is added in three times, adding manner is to be slowly added dropwise, during dropwise addition, since the surface of emulsified solution A is rich Collect prepolymer A, avoids leuco dye and acid regulator reaction solution.
Preferably, the leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane The mixture formed with weight ratio 14-18:0.6-1.4:0.4-1.
The leuco dye uses above-mentioned weight proportion, and three's synergistic effect improves the light resistance of leuco dye microcapsules, Guarantee the bright-coloured degree of color speed, tone and colour developing density simultaneously.
Preferably, the preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), 2-4 parts of styrene-maleic anhydride copolymers, 4-6 parts of esterification modification agent, 20-30 parts of first are weighed by weight Benzene and 0.05-0.2 parts of catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, is stirred evenly at 50-60 DEG C, then successively added Enter catalyst and esterification modification agent, 4-5h is stirred at 82-88 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- that mass fraction is 4-8% Aqueous solution.
Using esterification modification SMA made from above-mentioned preparation method, liquid phase surface tension can be reduced, facilitates leuco dye and exists Dispersion in water phase is effectively ensured stability of leuco dye during wall building, obtains the microcapsules of monoshell single wall, moreover it is possible to adjust It controls the prepolymer A being precipitated from water phase and is deposited on droplet surface, prepolymer A carries out polymerization reaction again and forms cyst wall, avoids pre-polymerization Object A generates blocky resin in water phase.SMA refers to styrene-maleic anhydride copolymer, further, the esterification modification agent For methanol, ethyl alcohol, n-butanol or n-octyl alcohol, the lipophilicity of SMA is improved, improves the binding force of esterification modification SMA and drop.Its In, in step (S2), stirring is dispersed in SMA in toluene at 50-60 DEG C, promotes esterification, and the catalyst is P-methyl benzenesulfonic acid reacts at 82-88 DEG C, improves reaction rate.
Preferably, the preparation method of every part of color developer microcapsule includes the following steps:
(B1) weighing 25-30 parts of color developing agents, 60-70 parts of turpentine oil, 40-50 parts of mass fractions by weight is 4-6%'s SMA- aqueous solution, 1-5 part nonionic surface active agent, 15-25 parts of urea, 35-45 parts of formaldehyde, 2-5 parts of acrylic acid-methyl-props Olefin(e) acid copolymer, 1-2 part defoaming agent and 10-15 parts of water, it is spare;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 50-60 DEG C, obtain chromogenic reagent solution;In 700- Under 900rpm revolving speed, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1300- 1600rpm, emulsion dispersion 1-2h obtain emulsified solution B, spare;
(B3) take urea, formaldehyde and acrylic acid-methacrylic acid copolymer mixing, be added alkaline conditioner adjust pH value to 7.5-9.5 stirs 0.5-2h, adds water uniformly mixed, obtain prepolymer B at a temperature of 50-80 DEG C, spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid Property regulator adjust pH value to 4-4.5,5-7h is stirred at 62-67 DEG C and stands 7-9h, color developer microcapsule is made in filtering.
Using color developer microcapsule made from above-mentioned preparation method, for particle diameter distribution at 0.4-12 μm, ball-type is complete, to core Completely, easy to leak, lustrous surface be not fine and close for capsule-core for material cladding.Wherein, step (B2) stirs at 50-60 DEG C promotes developer solution Solution improves production efficiency, under 700-900rpm revolving speed, chromogenic reagent solution is dispersed in SMA- aqueous solution in turpentine oil; The mass fraction of control SMA- aqueous solution is in 4-6%, insufficient in droplet surface if the mass fraction of SMA- aqueous solution is less than 4% To form the interfacial film of sufficient intensity, so that drop, which is mutually assembled, to become larger, the color developer microcapsule of preparation during wall building Partial size becomes larger, and particle size distribution range is wide, if the mass fraction of SMA- aqueous solution is greater than 6%, emulsion viscosity increases, poor fluidity, It is unfavorable for chromogenic reagent solution emulsion dispersion;The nonionic surface active agent of addition, stability is high, unionization in aqueous solution, Also not vulnerable to the influence of pH value, low foaming characteristic forms water-in-oil type (W/O) emulsion at a temperature of 50-60 DEG C, be conducive to it is pre- Polymers B is combined, and prepares the color developer microcapsule of lustrous surface densification.In step (B3), with acrylic acid-methacrylic acid copolymer For emulsifier, alkaline conditioner adjusts pH value and promotes urea and formaldehyde that condensation occurs anti-at a temperature of 50-80 DEG C to 7.5-9.5 Ureaformaldehyde performed polymer should be generated.In step (B4), defoaming agent is eliminated because the addition and stirring of nonionic surfactant lead to gas It steeps more, improves the regularity of color developer microcapsule;Acid regulator is added and adjusts pH value to 4-4.5, makes SMA- aqueous solution more Emulsification is effectively played, keeps droplet surface smooth, size droplet diameter narrow distribution range, partial size is small, while suitable prepolymer B's is anti- It answers, prepolymer B film-forming at 62-67 DEG C, if reaction temperature is too low, the surface porosity of the color developer microcapsule of formation is held Easily-deformable and leakage, if reaction temperature is excessively high, drop is easy, and bubble, the surface of the color developer microcapsule of formation are thick under stiring It is rough, it is easy mutually to be adhered.
Preferably, the color developing agent is alkyl salicylate zinc resin and/or phenolic resin;The non-ionic surfactant Agent is at least one of alkyl phenol polyoxyethylene ether, Tween-80 and fatty alcohol polyoxyethylene ether;The defoaming agent is At least one of BYK-052, BYK-080A and BYK-141.
It is furthermore preferred that the color developing agent is that alkyl salicylate zinc resin and phenolic resin are formed with weight ratio 5-8:1-4 Mixture, the two synergistic effect overcome the defect of alkyl salicylate zinc resin light resistance difference, and the hair of the balanced color developing agent of energy Color speed and colour developing density, improve the bright-coloured degree of tone, water resistance and the anti-yellowing property of color developing agent.The non-ionic table Face activating agent is alkyl phenol polyoxyethylene ether, Tween-80 and fatty alcohol polyoxyethylene ether with weight ratio 3-4:0.5-1:1-2 The mixture of composition under three's collective effect, significantly reduces the viscosity of drop, improves drop stability, promotes developer solution Balling-up and dispersion of the liquid in water phase, make the partial size of color developer microcapsule more evenly.The defoaming agent selects BYK-052, BYK- At least one of 080A and BYK-141, can in water-soluble solution, temperature is higher, remains to reach in acid stronger environment Play the role of stablizing defoaming.
In the present invention, the alkaline conditioner is in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate and ammonium hydroxide It is at least one;The acid regulator is acrylic acid.Preferably, the alkaline conditioner is sodium hydroxide, potassium hydroxide or ammonia Water is applied in preparing leuco dye microcapsules and color developer microcapsule, and regulating effect is fast, in step (A4) or step (B4) Bubble is not generated in acidization, can avoid, which influences wall building process, causes cyst wall deform, is soft or coarse.The acid regulator Acrylic acid is selected, in step (A4), avoids acidity too strong, hydrogen ion is excessively concentrated in acidization, and leuco dye is caused to mention Preceding colour developing, and avoid acidity too weak, the polymerization reaction of performed polymer A is incomplete, and cyst wall is soft;In step (B4), acrylic acid exists It is ionized at 62-67 DEG C, facilitates the solidification of performed polymer.
Another object of the present invention is achieved through the following technical solutions: a kind of preparation method of above-mentioned pressure detecting paper, Include the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant are weighed by weight And solvent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, are stirred at a temperature of 15-25 DEG C, under 50-100rmp revolving speed 1-2h is mixed, pressure-sensitive colour developing coating is made;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 5-15min, is made pressure detecting paper at 40-80 DEG C.
The present invention is using pressure detecting paper made from above-mentioned preparation method, and paper is smooth, any surface finish, coated on paper layer Pressure-sensitive color layer is not easy to lose powder, stain resistant, color inhibition, the density that develops the color and color development speed are preferable;The preparation method is easy to operate, Easy to control, high production efficiency, production cost is low, can be used for being mass produced.Wherein, in step (C2), in 15-25 DEG C of temperature Under, stir under 50-100rmp revolving speed, leuco dye microcapsules and color developer microcapsule expanded by heating are prevented, in high-speed stirred mistake Mutually collision causes rupture to develop the color in advance in journey.
The beneficial effects of the present invention are: pressure detecting paper of the invention, paper is smooth, any surface finish, is coated on paper layer Pressure-sensitive color layer be not easy to lose powder, stain resistant, color inhibition, develop the color density and color development speed it is preferable.It is replaced using color developer microcapsule It is coated on paper layer for the color developing agent of the prior art, improves the anti-yellowing property of color developing agent, and color developer microcapsule plays buffering pressure The effect of power, reduces the usage amount of interval dose, and the collective effect of color developer microcapsule and interval dose improves pressure detecting paper Compressive property avoids pressure detecting paper from damaging in use, and premature colouration causes paper to be scrapped;The surfactant of addition The wettability for improving pressure-sensitive color layer reduces the surface tension of pressure-sensitive color layer and improves the flatness of pressure-sensitive color layer, subtracts Delay because the use of color developer microcapsule and interval dose causes smoothness to lower, improves the quality of pressure detecting paper.
Preparation method of the invention is easy to operate, easy to control, and high production efficiency, production cost is low, can be used for extensive Production.
Specific embodiment
For the ease of the understanding of those skilled in the art, below with reference to embodiment, the present invention is further illustrated, real The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of pressure detecting paper including paper layer and is adhered to the pressure-sensitive color layer of paper layer, and the pressure-sensitive color layer is by such as The raw material of lower weight point is made:
The partial size of the leuco dye microcapsules is 2.2 μm, the leuco dye microcapsules, interval dose and the micro- glue of color developing agent The partial size ratio of capsule is 1:4:2.5.
The interval dose is calcium carbonate, and the adhesive is that carboxylic styrene butadiene latex and modified starch are mixed with weight ratio 1:2, The modified starch is oxidized starch.
It is 4:1 mixing, the solvent that the surfactant, which is sodium carboxymethylcellulose and methylcellulose with weight ratio, For water.
The preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) esterification modification that 3 parts of leuco dyes, 40 parts of solvent naphthas, 45 parts of mass fractions are 6% is weighed by weight SMA- aqueous solution, 30 parts of melamines, 17 parts of formaldehyde and 13 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 55 DEG C, obtain dye solution;In 1100rpm revolving speed Under, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 2000rpm, and emulsion dispersion 1.5h obtains emulsified solution A, it is spare;
(A3) melamine and formaldehyde is taken to be uniformly mixed, addition alkaline conditioner adjusting pH value is to 8, at a temperature of 65 DEG C, 1.5h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator It is acidified 1h, pH value is adjusted to 6.5, is warming up to 59 DEG C, continues to be acidified 0.5h, adjust pH value to 5.5, keep the temperature 1.8h, then adjust pH Value keeps the temperature 1.8h, stands 8h, leuco dye microcapsules are made in filtering to 4.5.
The leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane with weight ratio The mixture of 16:1:0.7 composition.
The preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), weigh by weight 3 parts of styrene-maleic anhydride copolymers, 5 parts of esterification modification agent, 25 parts of toluene and 0.12 part of catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, stirs evenly at 55 DEG C, then sequentially add 4.5h is stirred in catalyst and esterification modification agent at 85 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- water that mass fraction is 6% Solution.
Wherein, the esterification modification agent is ethyl alcohol, and the catalyst is p-methyl benzenesulfonic acid.
The preparation method of every part of color developer microcapsule includes the following steps:
(B1) the SMA- aqueous solution, 3 that 27 parts of color developing agents, 65 parts of turpentine oil, 45 parts of mass fractions are 5% are weighed by weight Part nonionic surface active agent, 20 parts of urea, 40 parts of formaldehyde, 3 parts of acrylic acid-methacrylic acid copolymers, 1.5 parts of defoaming agents It is spare with 12 parts of water;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 55 DEG C, obtain chromogenic reagent solution;In 800rpm revolving speed Under, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1450rpm, emulsion dispersion 1.5h obtains emulsified solution B, spare;
(B3) take urea, formaldehyde and acrylic acid-methacrylic acid copolymer mixing, be added alkaline conditioner adjust pH value to 8.5, at a temperature of 65 DEG C, 1.3h is stirred, adds water uniformly mixed, obtains prepolymer B, it is spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid Property regulator adjust pH value to 4.5, at 65 DEG C stir 6h stand 8h, filtering, be made color developer microcapsule.
The color developing agent is the mixture that alkyl salicylate zinc resin and phenolic resin are formed with weight ratio 7:3, described non- Ionic surfactant is alkyl phenol polyoxyethylene ether, Tween-80 and fatty alcohol polyoxyethylene ether with weight ratio 3.5: The mixture of 0.8:1.5 composition, the defoaming agent are BYK-052.
A kind of preparation method of pressure detecting paper as described above, includes the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant are weighed by weight And solvent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 1.5h at a temperature of 20 DEG C, under 75rmp revolving speed, Pressure-sensitive colour developing coating is made;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 10min, is made pressure detecting paper at 60 DEG C.
Embodiment 2
A kind of pressure detecting paper including paper layer and is adhered to the pressure-sensitive color layer of paper layer, and the pressure-sensitive color layer is by such as The raw material of lower weight point is made:
The partial size of the leuco dye microcapsules is 0.2 μm, the leuco dye microcapsules, interval dose and the micro- glue of color developing agent The partial size ratio of capsule is 1:3:2.
The interval dose is calcium carbonate, and the adhesive is that carboxylic styrene butadiene latex and modified starch are mixed with weight ratio 1:2, The modified starch is cationic starch.
It is 3:1 mixing, the solvent that the surfactant, which is sodium carboxymethylcellulose and methylcellulose with weight ratio, For water.
The preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) esterification modification that 1 part of leuco dye, 35 parts of solvent naphthas, 40 parts of mass fractions are 4% is weighed by weight SMA- aqueous solution, 25 parts of melamines, 10 parts of formaldehyde and 10 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 50 DEG C, obtain dye solution;In 900rpm revolving speed Under, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 1800rpm, and emulsion dispersion 1h obtains emulsified solution A, It is spare;
(A3) melamine and formaldehyde is taken to be uniformly mixed, addition alkaline conditioner adjusting pH value to 8, at 50 °C, 1h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator It is acidified 0.8h, pH value is adjusted to 6, is warming up to 58 DEG C, continues to be acidified 0.3h, adjust pH value to 5.0, keep the temperature 1.5h, then adjust pH Value keeps the temperature 1.5h, stands 7h, leuco dye microcapsules are made in filtering to 4.
The leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane with weight ratio The mixture of 14:0.6:0.4 composition.
The preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), weigh by weight 2 parts of styrene-maleic anhydride copolymers, 4 parts of esterification modification agent, 20 parts of toluene and 0.05 part of catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, stirs evenly at 50 DEG C, then sequentially add 4h is stirred in catalyst and esterification modification agent at 82 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- water that mass fraction is 4% Solution.
Wherein, the esterification modification agent is n-butanol, and the catalyst is p-methyl benzenesulfonic acid.
The preparation method of every part of color developer microcapsule includes the following steps:
(B1) the SMA- aqueous solution, 1 that 25 parts of color developing agents, 60 parts of turpentine oil, 40 parts of mass fractions are 4% are weighed by weight Part nonionic surface active agent, 15 parts of urea, 35 parts of formaldehyde, 2 parts of acrylic acid-methacrylic acid copolymers, 1 part of defoaming agent and 10 parts of water, it is spare;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 50 DEG C, obtain chromogenic reagent solution;In 700rpm revolving speed Under, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1300rpm, emulsion dispersion 1h obtains emulsified solution B, spare;
(B3) take urea, formaldehyde and acrylic acid-methacrylic acid copolymer mixing, be added alkaline conditioner adjust pH value to 7.5, at 50 °C, 0.5h is stirred, adds water uniformly mixed, obtains prepolymer B, it is spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid Property regulator adjust pH value to 4, at 62 DEG C stir 5h stand 7h, filtering, be made color developer microcapsule.
The color developing agent is the mixture that alkyl salicylate zinc resin and phenolic resin are formed with weight ratio 5:1, described non- Ionic surfactant is alkyl phenol polyoxyethylene ether, polysorbate and fatty alcohol polyoxyethylene ether with weight ratio 3:0.5:1 The mixture of composition, the defoaming agent are BYK-080A.
A kind of preparation method of pressure detecting paper as described above, includes the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant are weighed by weight And solvent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 1h at a temperature of 15 DEG C, under 50rmp revolving speed, make Obtain pressure-sensitive colour developing coating;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 5min, is made pressure detecting paper at 40 DEG C.
Embodiment 3
A kind of pressure detecting paper including paper layer and is adhered to the pressure-sensitive color layer of paper layer, and the pressure-sensitive color layer is by such as The raw material of lower weight point is made:
The partial size of the leuco dye microcapsules is 4 μm, the leuco dye microcapsules, interval dose and color developer microcapsule Partial size ratio be 1:5:3.
The interval dose is calcium carbonate, and the adhesive is that carboxylic styrene butadiene latex and modified starch are mixed with weight ratio 1:2, The modified starch is oxidized starch.
It is 5:1 mixing, the solvent that the surfactant, which is sodium carboxymethylcellulose and methylcellulose with weight ratio, For water.
The preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) esterification modification that 4 parts of leuco dyes, 45 parts of solvent naphthas, 50 parts of mass fractions are 8% is weighed by weight SMA- aqueous solution, 35 parts of melamines, 25 parts of formaldehyde and 15 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 60 DEG C, obtain dye solution;In 1300rpm revolving speed Under, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 2200rpm, and emulsion dispersion 2h obtains emulsified solution A, It is spare;
(A3) it takes melamine and formaldehyde to be uniformly mixed, alkaline conditioner is added and adjusts pH value to 8.5, in 80 DEG C of temperature Under, 2h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator It is acidified 1.2h, pH value is adjusted to 6.5, is warming up to 60 DEG C, continues to be acidified 0.6h, adjust pH value to 5.5, keep the temperature 1.2h, then adjust PH value keeps the temperature 1.2h, stands 9h, leuco dye microcapsules are made in filtering to 4.5.
The leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane with weight ratio The mixture of 18:1.4:1 composition.
The preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), 4 parts of styrene-maleic anhydride copolymers, 6 parts of esterification modification agent, 30 parts of toluene and 0.2 are weighed by weight Part catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, stirs evenly at 60 DEG C, then sequentially add 5h is stirred in catalyst and esterification modification agent at 88 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- water that mass fraction is 8% Solution.
Wherein, the esterification modification agent is n-octyl alcohol, and the catalyst is p-methyl benzenesulfonic acid.
The preparation method of every part of color developer microcapsule includes the following steps:
(B1) the SMA- aqueous solution, 5 that 30 parts of color developing agents, 70 parts of turpentine oil, 50 parts of mass fractions are 6% are weighed by weight Part nonionic surface active agent, 25 parts of urea, 45 parts of formaldehyde, 5 parts of acrylic acid-methacrylic acid copolymers, 2 parts of defoaming agents and 15 parts of water, it is spare;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 60 DEG C, obtain chromogenic reagent solution;In 900rpm revolving speed Under, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1600rpm, emulsion dispersion 2h obtains emulsified solution B, spare;
(B3) take urea, formaldehyde and acrylic acid-methacrylic acid copolymer mixing, be added alkaline conditioner adjust pH value to 9.5, at a temperature of 80 DEG C, 2h is stirred, adds water uniformly mixed, obtains prepolymer B, it is spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid Property regulator adjust pH value to 4.5, at 67 DEG C stir 7h stand 9h, filtering, be made color developer microcapsule.
The color developing agent is the mixture that alkyl salicylate zinc resin and phenolic resin are formed with weight ratio 8:4, described non- Ionic surfactant is alkyl phenol polyoxyethylene ether, Tween-80 and fatty alcohol polyoxyethylene ether with weight ratio 4:1:2 The mixture of composition, the defoaming agent are BYK-141.
A kind of preparation method of pressure detecting paper as described above, includes the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant are weighed by weight And solvent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 2h at a temperature of 25 DEG C, under 100rmp revolving speed, make Obtain pressure-sensitive colour developing coating;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 15min, is made pressure detecting paper at 80 DEG C.
Embodiment 4
A kind of pressure detecting paper including paper layer and is adhered to the pressure-sensitive color layer of paper layer, and the pressure-sensitive color layer is by such as The raw material of lower weight point is made:
The partial size of the leuco dye microcapsules is 3 μm, the leuco dye microcapsules, interval dose and color developer microcapsule Partial size ratio be 1:4.5:2.5.
The interval dose is silica sand;The adhesive is styrene-butadiene latex and propyl benzene latex and modified starch with weight ratio 1:2 Mixing.
The surfactant is sodium alginate;The solvent is ethyl alcohol.
The preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) esterification modification that 3 parts of leuco dyes, 42 parts of solvent naphthas, 42 parts of mass fractions are 5% is weighed by weight SMA- aqueous solution, 27 parts of melamines, 15 parts of formaldehyde and 11 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 53 DEG C, obtain dye solution;In 1000rpm revolving speed Under, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 1900rpm, and emulsion dispersion 1.8h obtains emulsified solution A, it is spare;
(A3) it takes melamine and formaldehyde to be uniformly mixed, alkaline conditioner is added and adjusts pH value to 8.5, in 75 DEG C of temperature Under, 1.8h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator Be acidified 1.1h, adjust pH value to 6, be warming up to 58 DEG C, continue to be acidified 0.5h, adjust pH value to 5, keep the temperature 16h, then adjust pH value to 4,1.6h is kept the temperature, 7.5h is stood, leuco dye microcapsules are made in filtering.
The leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane with weight ratio The mixture of 17:1.2:0.8 composition.
The preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), 2.5 parts of styrene-maleic anhydride copolymers, 4.5 parts of esterification modification agent, 23 parts of toluene are weighed by weight It is spare with 1 part of catalyst;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, stirs evenly at 53 DEG C, then sequentially add 4.2h is stirred in catalyst and esterification modification agent at 84 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- water that mass fraction is 5% Solution.
Wherein, the esterification modification agent is methanol, and the catalyst is p-methyl benzenesulfonic acid.
The preparation method of every part of color developer microcapsule includes the following steps:
(B1) the SMA- aqueous solution, 2 that 26 parts of color developing agents, 62 parts of turpentine oil, 42 parts of mass fractions are 4% are weighed by weight Part nonionic surface active agent, 18 parts of urea, 38 parts of formaldehyde, 3 parts of acrylic acid-methacrylic acid copolymers, 1.8 parts of defoaming agents It is spare with 13 parts of water;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 53 DEG C, obtain chromogenic reagent solution;In 850rpm revolving speed Under, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1400rpm, emulsion dispersion 1.8h obtains emulsified solution B, spare;
(B3) take urea, formaldehyde and acrylic acid-methacrylic acid copolymer mixing, be added alkaline conditioner adjust pH value to 8, at a temperature of 62 DEG C, 0.8h is stirred, adds water uniformly mixed, obtains prepolymer B, it is spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid Property regulator adjust pH value to 4, at 64 DEG C stir 6h stand 7h, filtering, be made color developer microcapsule.
The color developing agent is zinc salicylate resin;The nonionic surface active agent is alkyl phenol polyoxyethylene ether;Institute Stating defoaming agent is BYK-080A.
A kind of preparation method of pressure detecting paper as described above, includes the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant are weighed by weight And solvent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 1.8h at a temperature of 18 DEG C, under 80rmp revolving speed, Pressure-sensitive colour developing coating is made;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 9min, is made pressure detecting paper at 65 DEG C.Comparative example 1
A kind of pressure detecting paper, a kind of pressure detecting paper, including the paper layer, dye coating and developer layer being successively bonded, institute State the raw material that dye coating includes following weight point:
The partial size of the leuco dye microcapsules is 2.2 μm, and the partial size ratio of the leuco dye microcapsules and interval dose is 1:4.
The interval dose is calcium carbonate, and the adhesive is that carboxylic styrene butadiene latex and modified starch are mixed with weight ratio 1:2, The modified starch is oxidized starch.
It is 4:1 mixing, the solvent that the surfactant, which is sodium carboxymethylcellulose and methylcellulose with weight ratio, For water.
The preparation method of every part of leuco dye microcapsules includes the following steps:
(A1) esterification modification that 3 parts of leuco dyes, 40 parts of solvent naphthas, 45 parts of mass fractions are 6% is weighed by weight SMA- aqueous solution, 30 parts of melamines, 17 parts of formaldehyde and 13 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 55 DEG C, obtain dye solution;In 1100rpm revolving speed Under, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 2000rpm, and emulsion dispersion 1.5h obtains emulsified solution A, it is spare;
(A3) melamine and formaldehyde is taken to be uniformly mixed, addition alkaline conditioner adjusting pH value is to 8, at a temperature of 65 DEG C, 1.5h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator It is acidified 1h, pH value is adjusted to 6.5, is warming up to 59 DEG C, continues to be acidified 0.5h, adjust pH value to 5.5, keep the temperature 1.8h, then adjust pH Value keeps the temperature 1.8h, stands 8h, leuco dye microcapsules are made in filtering to 4.5.
The leuco dye is by crystal violet lactone, Bengoyl Leuco Methylene Blue and diaryl carbazole methane with weight ratio The mixture of 16:1:0.7 composition.
The preparation method of every part of esterification modification SMA- aqueous solution includes the following steps:
(S1), weigh by weight 3 parts of styrene-maleic anhydride copolymers, 5 parts of esterification modification agent, 25 parts of toluene and 0.12 part of catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, stirs evenly at 55 DEG C, then sequentially add 4.5h is stirred in catalyst and esterification modification agent at 85 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), prepare the esterification modification SMA- water that mass fraction is 6% Solution.
Wherein, the esterification modification agent is ethyl alcohol, and the catalyst is p-methyl benzenesulfonic acid.
The developer layer is the mixture that alkyl salicylate zinc resin and phenolic resin are formed with weight ratio 7:3.
A kind of preparation method of pressure detecting paper as described above, includes the following steps:
(C1) leuco dye microcapsules, interval dose, adhesive, surfactant and solvent are weighed by weight, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 1.5h at a temperature of 20 DEG C, under 75rmp revolving speed, Pressure-sensitive colour developing coating is made;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 10min, is coated with developer layer at 60 DEG C, and pressure is made Power detects paper.
The performance test of 5 pressure detecting paper of embodiment
Example 1-4 and the pressure detecting paper of comparative example 1 carry out color inhibition, smoothness and minimum pressure colour developing respectively and survey Examination.
Test method is as follows:
Color inhibition test method: taking pressure detecting paper, is cut into the sample of 50mm × 12mm, and a sample is stayed to make blank, It is remaining to be placed in HZ-3017 type bulb-type color inhibition experimental box, carry out illumination for 24 hours under the ultraviolet lamp of 300W, sample and light bulb away from From the temperature 60 C or so for 25cm, in exposure box.Experimental period to be reached takes out cooling 10min or more, then observes its Huang Denaturation, and its color is compared on grey colour atla with blank sample, test mode meets GB250-1995.
Smoothness test method: using Buick smoothness instrument at vacuum degree 80kPa, the air capacity of 5m3 is made to exist Pass through the time needed for the gap between specimen surface and glass surface under 100kPa pressure.
Minimum pressure colour developing test method: applying the pressure of n × 10KPa to pressure detecting paper, and n indicates what pressure extremely developed the color Number.
Test result is as follows shown in table 1.
Table 1
Test index Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Comparative example 1
Xanthochromia grade 5 4-5 5 5 2
Smoothness (s) 67 69 61 64 57
Pressure colour developing test (n) 20 23 18 19 10
As seen from the above table, the anti-yellowing property of comparative example 1 is poor, and significantly improves yellowing resistance using color developer microcapsule Energy;Because pressure-sensitive color layer of the invention contains interval dose, color developer microcapsule and leuco dye microcapsules, the partial size of three is different, But it can fill close, while cooperate other auxiliary agents, the smoothness of pressure detecting paper of the invention is made to reach 61-69s, and due to The surface layer of comparative example 1 is developer layer, and the surface smoothness after coating is lower than the smoothness of pressure detecting paper of the invention;This The minimum pressure color range for inventing the pressure detecting paper of preparation is 180-230KPa, more anti-than the pressure detecting paper of comparative example 1 It presses performance good, avoids pressure detecting paper from damaging in use, premature colouration causes paper to be scrapped.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other way, Do not depart under the premise of present inventive concept it is any obviously replace it is within the scope of the present invention.

Claims (10)

1. a kind of pressure detecting paper, it is characterised in that: including paper layer and it is adhered to the pressure-sensitive color layer of paper layer, it is described pressure-sensitive aobvious Chromatograph is made by the raw material of following weight point:
2. a kind of pressure detecting paper according to claim 1, it is characterised in that: the partial size of the leuco dye microcapsules is 0.2-4 μm, the partial size ratio of the leuco dye microcapsules, interval dose and color developer microcapsule is 1:3-5:2-3.
3. a kind of pressure detecting paper according to claim 1, it is characterised in that: the interval dose is starch, silica sand, junket egg At least one of white, kaolin and calcium carbonate;The adhesive is styrene-butadiene latex, carboxylic styrene butadiene latex, propyl benzene latex and changes At least one of property starch.
4. a kind of pressure detecting paper according to claim 1, it is characterised in that: the surfactant be sodium alginate, At least one of sodium carboxymethylcellulose and methylcellulose;The solvent is water or ethyl alcohol.
5. a kind of pressure detecting paper according to claim 1, it is characterised in that: the system of every part of leuco dye microcapsules Preparation Method includes the following steps:
(A1) esterification that 1-4 parts of leuco dyes, 35-45 parts of solvent naphthas, 40-50 parts of mass fractions are 4-8% is weighed by weight Modified SMA- aqueous solution, 25-35 parts of melamines, 10-25 parts of formaldehyde and 10-15 parts of water, it is spare;
(A2) it takes leuco dye and solvent naphtha to mix, is stirred evenly at 50-60 DEG C, obtain dye solution;Turn in 900-1300rpm Under speed, dye solution is added into esterification modification SMA- aqueous solution, revolving speed is adjusted to 1800-2200rpm, and emulsion dispersion 1-2h is obtained Emulsified solution A, it is spare;
(A3) it takes melamine and formaldehyde to be uniformly mixed, alkaline conditioner is added and adjusts pH value to 8-8.5, in 50-80 DEG C of temperature Under, 1-2h is stirred, adds water uniformly mixed, obtains prepolymer A, it is spare;
(A4) the prepolymer A mixing of step (A3) is added into the emulsified solution A of step (A2), adds acid regulator acidification 0.8-1.2h adjusts pH value to 6-6.5, is warming up to 58-60 DEG C, continues to be acidified 0.3-0.6h, adjust pH value to 5.0-5.5, protect Warm 1.5-2h, then pH value is adjusted to 4-4.5,1.5-2h is kept the temperature, 7-9h is stood, leuco dye microcapsules are made in filtering.
6. a kind of pressure detecting paper according to claim 5, it is characterised in that: the leuco dye is by crystal violet The mixture that ester, Bengoyl Leuco Methylene Blue and diaryl carbazole methane are formed with weight ratio 14-18:0.6-1.4:0.4-1.
7. a kind of pressure detecting paper according to claim 5, it is characterised in that: every part of esterification modification SMA- aqueous solution Preparation method include the following steps:
(S1), weigh by weight 2-4 parts of styrene-maleic anhydride copolymers, 4-6 parts of esterification modification agent, 20-30 parts of toluene and 0.05-0.2 parts of catalyst, it is spare;
(S2), it takes toluene and styrene-maleic anhydride copolymer to mix, is stirred evenly at 50-60 DEG C, then sequentially add and urge 4-5h is stirred in agent and esterification modification agent at 82-88 DEG C, filters, drying, esterification modification SMA is made;
(S3), add water into the esterification modification SMA of step (S2), it is water-soluble to prepare the esterification modification SMA- that mass fraction is 4-8% Liquid.
8. a kind of pressure detecting paper according to claim 1, it is characterised in that: the preparation of every part of color developer microcapsule Method includes the following steps:
(B1) SMA- that 25-30 parts of color developing agents, 60-70 parts of turpentine oil, 40-50 parts of mass fractions are 4-6% is weighed by weight Aqueous solution, 1-5 part nonionic surface active agent, 15-25 parts of urea, 35-45 parts of formaldehyde, 2-5 parts of acrylic acid-methacrylic acids Copolymer, 1-2 part defoaming agent and 10-15 parts of water, it is spare;
(B2) it takes color developing agent and turpentine oil to mix, is stirred evenly at 50-60 DEG C, obtain chromogenic reagent solution;Turn in 700-900rpm Under speed, chromogenic reagent solution is added into SMA- aqueous solution and nonionic surface active agent, revolving speed are adjusted to 1300-1600rpm, cream Change dispersion 1-2h, obtains emulsified solution B, it is spare;
(B3) urea, formaldehyde and the mixing of acrylic acid-methacrylic acid copolymer are taken, alkaline conditioner is added and adjusts pH value to 7.5- 9.5, at a temperature of 50-80 DEG C, 0.5-2h is stirred, adds water uniformly mixed, obtains prepolymer B, it is spare;
(B4) the prepolymer B mixing of defoaming agent and step (B3) is added into the emulsified solution B of step (B2), adds acid tune It saves agent and adjusts pH value to 4-4.5,5-7h is stirred at 62-67 DEG C and stands 7-9h, color developer microcapsule is made in filtering.
9. a kind of pressure detecting paper according to claim 8, it is characterised in that: the color developing agent is alkyl salicylate zinc tree Rouge and/or phenolic resin;The nonionic surface active agent is alkyl phenol polyoxyethylene ether, Tween-80 and fatty alcohol At least one of polyoxyethylene ether;The defoaming agent is at least one of BYK-052, BYK-080A and BYK-141.
10. a kind of preparation method of pressure detecting paper as described in any one of claims 1-9, it is characterised in that: including such as Lower step:
(C1) leuco dye microcapsules, interval dose, adhesive, color developer microcapsule, surfactant and molten are weighed by weight Agent, it is spare;
(C2) other raw materials of step (C1) are added into solvent, stir 1- at a temperature of 15-25 DEG C, under 50-100rmp revolving speed Pressure-sensitive colour developing coating is made in 2h;
(C3) pressure-sensitive colour developing coating is coated on paper layer, dry 5-15min, is made pressure detecting paper at 40-80 DEG C.
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