CN106590150B - Aluminum powder pigment for steaming-resistant ink and preparation method thereof - Google Patents

Aluminum powder pigment for steaming-resistant ink and preparation method thereof Download PDF

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CN106590150B
CN106590150B CN201710000733.9A CN201710000733A CN106590150B CN 106590150 B CN106590150 B CN 106590150B CN 201710000733 A CN201710000733 A CN 201710000733A CN 106590150 B CN106590150 B CN 106590150B
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aluminum powder
pigment
aluminum
phosphate ester
powder pigment
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CN106590150A (en
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石龙
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Zuxing New Material Co ltd
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Zuxing New Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
    • C09D11/037Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment

Abstract

The invention discloses an aluminum powder pigment for steam-resistant ink and a preparation method thereof, wherein the aluminum powder pigment for steam-resistant ink comprises aluminum powder and a phosphate ester auxiliary agent adsorbed on the aluminum powder pigment, and the mass ratio of the aluminum powder to the phosphate ester auxiliary agent is 1: (0.01-0.1), and the phosphate ester auxiliary agent is alkyl phosphate ester. The aluminum powder pigment for the steam-resistant ink has a large amount of hydroxyl groups on the surface of aluminum powder, and the hydroxyl groups can adsorb phosphate ester auxiliary agents, so that the aluminum powder is isolated from contacting corrosive environment media such as water, air and the like, and a formed paint film is steam-resistant, does not fade and does not fall off.

Description

Aluminum powder pigment for steaming-resistant ink and preparation method thereof
Technical Field
The invention relates to the field of aluminum pigments for ink, in particular to an aluminum powder pigment for steaming-resistant ink. In addition, the invention also relates to a preparation method of the aluminum powder pigment for the steaming-resistant ink.
Background
The aluminum pigment for the ink comprises slurry, powder and strip products, is an important component of the aluminum pigment, and is also a high-value variety. The product is required to have a fine particle size, a high covering power and good dispersibility. For the aluminum pigment applied to food packaging ink and cigarette packet products, various environmental requirements are also required, such as no triphenyl, plasticizer, various heavy metals and the like. Particularly, on the basis of meeting the above conditions, the ink paint film is also required to be steamed and boiled for 40 minutes at 121 ℃, and the paint film does not fall off or change color. With the development of the food industry, more and more products are produced, and therefore, the use amount of the products is increased. At present, however, there are few manufacturers of aluminum pigments that can produce such products. According to the information mastered at present, only two or three companies such as schlenk and the like have products to meet the requirements, and no product of a manufacturer at home can meet the requirements. Therefore, it is necessary to develop such products and to establish the serialization.
Disclosure of Invention
The invention provides an aluminum powder pigment for steaming-resistant ink and a preparation method thereof, which aim to solve the technical problem of high-temperature steaming resistance of an ink paint film.
The technical scheme adopted by the invention is as follows:
the invention provides an aluminum powder pigment for steaming-resistant ink, which comprises aluminum powder and a phosphate ester auxiliary agent adsorbed on the aluminum powder pigment, wherein the mass ratio of the aluminum powder to the phosphate ester auxiliary agent is 1: (0.01-0.1), and the phosphate ester auxiliary agent is alkyl phosphate ester.
Further, the mass ratio of the aluminum powder pigment to the phosphate ester auxiliary agent is 1: 0.03, the phosphate ester auxiliary agent is octyl phosphate ester, hexyl phosphate ester or butyl phosphate ester, and preferably, the phosphate ester auxiliary agent is hexyl phosphate ester.
The invention also provides a preparation method of the aluminum powder pigment for the steaming-resistant ink, which comprises the following steps:
dispersing the clean aluminum powder pigment in a first solvent, adding the phosphate ester auxiliary agent into the first solvent in batches, and stirring.
And filtering and drying the prepared mixed solution to obtain the aluminum powder pigment for the steaming-resistant ink.
Wherein the mass ratio of aluminum to the phosphate ester auxiliary agent in the clean aluminum powder pigment is 1: (0.01-0.1), and the phosphate ester auxiliary agent is alkyl phosphate ester.
Further, in the step of adding the phosphate ester auxiliary agent, the temperature is controlled to be 38-42 ℃, and preferably 40 ℃.
Further, vacuum filtration is adopted for the mixed solution, and the drying temperature is 50-90 ℃, preferably 80 ℃.
And further dissolving the phosphate ester auxiliary agent in a second solvent, and then dropwise adding the phosphate ester auxiliary agent into the first solvent containing the clean aluminum powder pigment, wherein the stirring time is 3-5 hours.
Furthermore, the second solvent is the same as the first solvent, and is an ether solvent, and the ether solvent is propylene glycol methyl ether.
Further, the preparation of the pure aluminum pigment comprises the following steps:
uniformly mixing the aluminum pigment with an ether solvent or an alcohol solvent which is 2-6 times the mass of the aluminum pigment, stirring for 3-5 hours at 28-32 ℃, removing impurity oil in the aluminum pigment, filtering, and keeping the solid content at 60 +/-2% to obtain the clean aluminum powder pigment. Preferably, the aluminum pigment is mixed with an ether solvent, wherein the ether solvent is propylene glycol methyl ether.
Further, the step of cleaning the aluminum powder pigment dispersed in the first solvent includes:
uniformly stirring 10-20 parts by weight of clean aluminum powder pigment and 20-50 parts by weight of ether solvent.
Further, the step of sieving by a 200-mesh sieve is also included after the drying.
The invention has the following beneficial effects: the aluminum powder pigment for the steam-resistant ink has a large amount of hydroxyl groups on the surface of aluminum powder, and the hydroxyl groups can adsorb phosphate ester auxiliary agents, so that the aluminum powder is isolated from contacting corrosive environment media such as water, air and the like, and a formed paint film is steam-resistant, does not fade and does not fall off.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below with reference to the drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a diagram of a retort-resistant ink according to a preferred embodiment 3 of the present invention before retort processing with an aluminum powder pigment-coated PT film;
FIG. 2 is a diagram of a retort-resistant ink of a preferred embodiment 3 of the present invention after being cooked with a PT film coated with an aluminum powder pigment;
FIG. 3 is a diagram of a retort-resistant ink of a preferred embodiment 4 of the present invention before retort processing with an aluminum powder pigment coated PT film;
FIG. 4 is a diagram of a retort-resistant ink of preferred embodiment 4 of the present invention after retort processing with a PT film coated with an aluminum powder pigment.
Detailed Description
The embodiments of the invention will be described in detail below with reference to the drawings, but the invention can be implemented in many different ways as defined and covered by the claims.
Referring to fig. 1, a preferred embodiment of the present invention provides an aluminum powder pigment for retort ink, including aluminum powder and a phosphate ester assistant adsorbed on the aluminum powder pigment, wherein the mass ratio of the aluminum powder to the phosphate ester assistant is 1: (0.01-0.1), and the phosphate ester auxiliary agent is alkyl phosphate ester.
Aluminum pigments are fine aluminum powders generally prepared by liquid processes such as sanding in a liquid. Therefore, the aluminum pigment usually contains impurity oil, which affects the coating of the aluminum pigment. The aluminum powder for the aluminum powder pigment for the steaming-resistant ink is dry aluminum pigment with impurity oil removed usually, or fine aluminum particles which are directly prepared by other preparation methods and do not contain other impurities. The aluminum powder particles may be the same size as the aluminum powder particles in a general aluminum pigment. The mass of the aluminum powder is measured as dry pure aluminum powder.
The phosphate ester auxiliary agent is alkyl phosphate ester. The aluminum alloy has good stability, and can isolate aluminum from corrosive environment media such as water, air and the like. So that a paint film formed by the aluminum powder is resistant to boiling, does not fade and does not fall off. The mass ratio of the aluminum powder to the phosphate ester auxiliary agent is 1: (0.01-0.1).
The invention has the following beneficial effects: the aluminum powder pigment for the steam-resistant ink has a large amount of hydroxyl groups on the surface of aluminum powder, and the hydroxyl groups can adsorb phosphate ester auxiliary agents, so that the aluminum powder is isolated from contacting corrosive environment media such as water, air and the like, and a formed paint film is steam-resistant, does not fade and does not fall off.
Optionally, the mass ratio of the aluminum powder pigment to the phosphate ester assistant is 1: 0.03, the phosphate ester auxiliary agent is octyl phosphate ester, hexyl phosphate ester or butyl phosphate ester, and preferably, the phosphate ester auxiliary agent is hexyl phosphate ester. The stability of the octyl phosphate, the hexyl phosphate or the butyl phosphate is good, and the prepared aluminum powder pigment has more stable performance, better cooking resistance effect and less fading. Among them, hexyl phosphate is most effective.
The invention also provides a preparation method of the aluminum powder pigment for the steaming-resistant ink, which comprises the following steps:
dispersing clean aluminum powder pigment in a first solvent, adding phosphate ester auxiliary agent in batches, and stirring;
and filtering and drying the prepared mixed solution to obtain the aluminum powder pigment for the steaming-resistant ink.
Wherein the mass ratio of aluminum to the phosphate ester auxiliary agent of the clean aluminum powder pigment is 1: (0.01-0.1), and the phosphate ester auxiliary agent is alkyl phosphate ester.
The clean aluminum pigment is an aluminum pigment with impurity oil removed, may or may not contain a solvent, and is dry pure aluminum powder. The clean aluminum pigment and the first solvent can be added into a reaction vessel, and can be uniformly dispersed by stirring, shaking or ultrasonic waves. The phosphate ester adjuvant may be added to the reaction vessel in portions.
The aluminum pigment has a large number of hydroxyl groups on the surface:
Al+xH2O→[Al(OH)x](3-x)++xH+
optionally, in the step of adding the phosphate ester auxiliary agent, the temperature is controlled to be 38-42 ℃, and preferably 40 ℃.
When the temperature is too low, the speed of adsorbing the phosphate auxiliary agent by the aluminum powder in the clean aluminum pigment is too low, the thickness of the phosphate auxiliary agent layer is relatively thin, and the prepared aluminum powder pigment for the steaming-resistant ink is poor in steaming resistance. When the temperature is too high, the speed of adsorbing the phosphate auxiliary by the aluminum powder is too high, and the phosphate auxiliary layer coated outside the aluminum powder is too thick, so that the aluminum powder particles are coarse, and the color difference of a paint film formed by the aluminum powder pigment for the steaming-resistant ink is poor, and is specifically represented by poor metal feeling and poor covering power. Therefore, in the process of adding the phosphate ester auxiliary agent, the temperature of the reaction system is controlled to be 38-42 ℃, and more preferably 40 ℃.
Optionally, the mixed solution is subjected to vacuum filtration, and the drying temperature is 50-90 ℃, preferably 80 ℃.
When the drying temperature is too low, the drying time is undoubtedly increased, and the production efficiency is reduced. When the drying temperature is too high, the aluminum powder pigment for the steaming and boiling resistant ink is easy to agglomerate, the hue of a paint film is reduced, and the metallic feeling and the covering power are poor.
Optionally, after the phosphate ester auxiliary agent is dissolved in the second solvent, the phosphate ester auxiliary agent is dripped into the first solvent containing the clean aluminum powder pigment, and the stirring time is 3-5 hours.
The second solvent and the first solvent may be the same or different. The phosphate ester auxiliary agent is dissolved in the second solvent and slowly dripped into the first solvent containing the clean aluminum powder pigment, so that the adsorption speed of the aluminum powder can be better controlled, and the charging is more uniform. The stirring time is too short, so that the reaction is insufficient, the product can not meet the requirement of steaming resistance, the stirring time is too long, so that the reaction is excessive, the phosphate ester auxiliary agent layer coated outside the aluminum powder is too thick, the aluminum powder particles are coarse, and the paint film formed by the aluminum powder pigment for the steaming resistance ink has poor color difference, which is concretely represented by poor metal feeling and poor covering power.
Optionally, the second solvent is the same as the first solvent, and both are ether solvents, and the ether solvent is propylene glycol methyl ether. The second solvent is the same as the first solvent, so that the aluminum powder can be conveniently dispersed. Meanwhile, the propylene glycol methyl ether has good dispersibility, so that the aluminum powder is uniformly dispersed, and the aluminum powder pigment for the steaming-resistant ink has fine particles and better hue.
Alternatively, the preparation of the pure aluminum pigment comprises the following steps:
uniformly mixing the aluminum pigment with an ether solvent or an alcohol solvent which is 2-6 times the mass of the aluminum pigment, stirring for 3-5 hours at 28-32 ℃, removing impurity oil in the aluminum pigment, filtering, and keeping the solid content at 60 +/-2% to obtain the clean aluminum powder pigment. Preferably, the aluminum pigment is mixed with an ether solvent, wherein the ether solvent is propylene glycol methyl ether.
Aluminum pigments are fine aluminum powders, typically prepared by liquid processes such as sanding in a liquid. Therefore, the aluminum pigment usually contains impurity oil. The impure oil is mixed with an ether solvent and can be removed by filtration. The aluminum pigment can be dispersed in ether solvent or alcohol solvent to remove impurity oils such as ethanol and propylene glycol methyl ether. In contrast, the aluminum powder pigment particles for the steaming-resistant ink prepared by using the ethanol as the solvent are relatively larger and have relatively poor dispersibility compared with the aluminum powder pigment particles prepared by using propylene glycol methyl ether as the solvent.
Optionally, the step of cleaning the aluminum flake pigment dispersed in the first solvent comprises:
uniformly stirring 10-20 parts by weight of clean aluminum powder pigment and 20-50 parts by weight of ether solvent.
Optionally, the step of sieving with a 200-mesh sieve is further included after drying.
The aluminum powder pigment for the steaming and boiling resistant ink with the particle size of-200 meshes is obtained by screening, and has strong metal feeling and excellent comprehensive performance.
Example 1
1. According to the mass fraction, 10 parts of aluminum pigment and 60 parts of ether solvent are uniformly mixed, after stirring for 3 hours at 28 ℃, impurity oil in the aluminum pigment is removed, and the mixture is subjected to suction filtration by a vacuum pump, so that the solid content is kept at 58%.
2. Adding 10 parts of the filter cake prepared in the step 1 and 20 parts of the ether solvent into a reaction container according to the mass fraction, and uniformly stirring.
3. 0.1 part of caprylocaproyl phosphate was dissolved in 0.5 part of an ether solvent, and after uniformly mixing, the solution was slowly dropped into a reaction vessel, and stirred for 3 hours while the temperature was maintained at 38 ℃.
4. And (4) carrying out suction filtration on the solution prepared in the step (3) by using a vacuum pump, drying in a 50 ℃ oven, and screening by using a 200-mesh screen to obtain the aluminum powder pigment for the steaming-resistant ink.
Example 2
1. According to the mass fraction, 15 parts of aluminum pigment and 45 parts of ether solvent are uniformly mixed, stirred for 4 hours at the temperature of 30 ℃, impurity oil in the aluminum pigment is removed, and the aluminum pigment is subjected to suction filtration by a vacuum pump, so that the solid content is kept at 60%.
2. Adding 15 parts of the filter cake prepared in the step 1 and 30 parts of the ether solvent into a reaction container according to the mass fraction, and uniformly stirring.
3. 0.3 part of butyl phosphate was dissolved in 1 part of an ether solvent, and after uniformly mixing, the mixture was slowly dropped into a reaction vessel and stirred for 4 hours, with the temperature being maintained at 39 ℃.
4. And (4) carrying out suction filtration on the solution prepared in the step (3) by using a vacuum pump, drying in a 60 ℃ oven, and screening by using a 200-mesh screen to obtain the aluminum powder pigment for the steaming-resistant ink.
Example 3
1. According to the mass fraction, 18 parts of aluminum pigment and 55 parts of ether solvent are uniformly mixed, stirred for 4.5 hours at 31 ℃, impurity oil in the aluminum pigment is removed, and the aluminum pigment is filtered by a vacuum pump, so that the solid content is kept at 61%.
2. Adding 18 parts of the filter cake prepared in the step 1 and 30 parts of the ether solvent into a reaction container according to the mass fraction, uniformly stirring,
3. 0.3 part of hexyl phosphate is dissolved in 1.5 parts of ether solvent, mixed uniformly, and slowly dropped into a reaction vessel, stirred for 4.5 hours, and the temperature is kept at 40 ℃.
4. And (4) carrying out suction filtration on the solution prepared in the step (3) by using a vacuum pump, drying in an oven at the temperature of 80 ℃, and screening by using a 200-mesh screen to obtain the aluminum powder pigment for the steaming-resistant ink.
Example 4
1. According to the mass fraction, 20 parts of aluminum pigment and 40 parts of ether solvent are uniformly mixed, stirred for 4 hours at the temperature of 30 ℃, impurity oil in the aluminum pigment is removed, and the aluminum pigment is filtered by a vacuum pump, so that the solid content is kept at 62%.
2. Adding 20 parts of the filter cake prepared in the step 1 and 50 parts of the ether solvent into a reaction container according to the mass fraction, and uniformly stirring.
3. 0.4 part of caprylocaproyl phosphate was dissolved in 2 parts of an ether solvent, and after uniformly mixing, the solution was slowly dropped into a reaction vessel, and stirred for 5 hours while the temperature was maintained at 42 ℃.
4. And (4) carrying out suction filtration on the solution prepared in the step (3) by using a vacuum pump, drying in a drying oven at 90 ℃, and screening by using a 200-mesh screen to obtain the aluminum powder pigment for the steaming-resistant ink.
The aluminum powder pigments for the retort resistant inks of examples 1 to 4 were prepared into paints and then scraped on different PT films. The PT films corresponding to examples 1 to 4 were placed in a back-pressure high-temperature digester device and cooked at 121 ℃ under 2 atmospheres for 40 minutes. And after the cooking is finished, taking out the product to observe the paint film effect. The PT films corresponding to the embodiments 1-4 have good color and good paint film without falling off or color change.
As shown in fig. 1-4. The aluminum powder pigments for the retort resistant inks of examples 3 and 4 were respectively made into paints and scraped on different PT films, and before and after retort, the paint films were not greatly different and were not peeled off or discolored.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. The preparation method of the aluminum powder pigment for the steaming-resistant ink is characterized by comprising the following steps of:
uniformly mixing an aluminum pigment and an ether solvent with the mass being 2-6 times that of the aluminum pigment, stirring for 3-5 hours at 28-32 ℃, removing impurity oil in the aluminum pigment, filtering, and keeping the solid content at 60 +/-2% to obtain a clean aluminum powder pigment;
uniformly stirring 10-20 parts by weight of clean aluminum powder pigment and 20-50 parts by weight of first solvent, dissolving phosphate ester auxiliary agent in a second solvent, dropwise adding the phosphate ester auxiliary agent into the first solvent containing the clean aluminum powder pigment at 40 ℃, stirring for 3-5 hours, wherein the second solvent is the same as the first solvent and is propylene glycol methyl ether;
filtering the prepared mixed solution, and drying at 50-90 ℃ to obtain aluminum powder pigment for the steaming-resistant ink;
wherein the mass ratio of the aluminum in the clean aluminum powder pigment to the phosphate ester auxiliary agent is 1: (0.01-0.1), and the phosphate ester auxiliary agent is hexyl phosphate ester.
2. The method for preparing the aluminum powder pigment for the steam resistant ink as claimed in claim 1, wherein the mixed solution is vacuum filtered and dried at 80 ℃.
3. The method for preparing the aluminum powder pigment for the retort ink according to claim 1 or 2, further comprising a step of sieving with a 200-mesh sieve after drying.
CN201710000733.9A 2017-01-03 2017-01-03 Aluminum powder pigment for steaming-resistant ink and preparation method thereof Active CN106590150B (en)

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Denomination of invention: Aluminum powder pigment for cooking resistant ink and its preparation method

Effective date of registration: 20210918

Granted publication date: 20200814

Pledgee: Ningxiang sub branch of Bank of Changsha Co.,Ltd.

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