Water-based ceramic glaze ink with high stability and preparation method thereof

Abstract

The invention provides water-based ceramic glaze ink with high stability, which is prepared from the following ingredients in parts by weight: 40 to 80 parts of ceramic glaze particles, 3 to 6 parts of first dispersing agents, 2 to 7 parts of second dispersing agents, 1 to 4 parts of stabilizing agents, 0.5 to 2 parts of anti-settling agents, 2 to 4 parts of surfactants and 60 to 100 parts of water. In the preparation process of the water-based ceramic glaze ink, a first dispersing agent, a second dispersing agent, a stabilizer, an anti-settling agent, a surfactant and the like are introduced into ceramic glaze particles serving as a matrix, so that the dispersion stability, surface tension and other properties are greatly improved.

Description

Technical Field

[0001] The invention belongs to the technical field of glaze inks, and specifically relates to a water-based ceramic glaze ink with high stability and a preparation method thereof. Background Art

[0002] Water-based ceramic glaze ink is a type of ink specifically used for ceramic printing, which uses water as a solvent or dispersion medium. Compared with traditional oil-based or solvent-based inks, water-based ceramic glaze inks are environmentally friendly, low-odor, and safer during the printing process. This type of ink usually contains the following components: Pigments or colorants: basic components that provide color; Binders: ensure that the ink can firmly adhere to the ceramic surface; Dispersants and stabilizers: help the pigments to disperse evenly and prevent precipitation; Water or other solvents: as a carrier, it is convenient for the ink to be sprayed and dried. Water-based ceramic glaze inks have a wide range of applications and can be used to decorate various ceramic products such as tableware, tiles, etc. Through digital inkjet technology, high-precision and diversified pattern printing can be achieved on the ceramic surface.

[0003] The performance of ceramic inkjet printing ink is mainly determined by the dispersibility of the ceramic phase (solid phase) and its suspension stability. Currently, most water-based inks on the market are pigment inks, which have the disadvantages of low solid content, small inkjet volume, poor color development effect, and stain resistance. In particular, there is a lot of room for improvement in glaze viscosity, surface tension, and dispersion stability. Therefore, it is particularly important to develop a highly stable water-based ceramic glaze ink for this type of product application. Summary of the invention

[0004] The purpose of the present invention is to provide a water-based ceramic glaze ink with high stability and a preparation method thereof, by introducing a first dispersant, a second dispersant, a stabilizer, an anti-settling agent, a surfactant, etc. into the ceramic glaze particles as a matrix to greatly improve the dispersion stability, surface tension and other properties.

[0005] In order to achieve the above object, the present invention provides the following technical solutions: A highly stable water-based ceramic glaze ink comprises the following components by weight: 40-80 parts of ceramic glaze particles, 3-6 parts of a first dispersant, 2-7 parts of a second dispersant, 1-4 parts of a stabilizer, 0.5-2 parts of an anti-settling agent, 2-4 parts of a surfactant, and 60-100 parts of water.

[0006] Furthermore, the following components are included in parts by weight: 65 parts of ceramic glaze particles, 5 parts of a first dispersant, 4.5 parts of a second dispersant, 2.5 parts of a stabilizer, 1 part of an anti-settling agent, 3 parts of a surfactant, and 85 parts of water.

[0007] Furthermore, the surfactant is fatty alcohol polyoxyethylene ether.

[0008] The method for preparing the above-mentioned water-based ceramic glaze ink with high stability comprises the following steps: S1: preparing ceramic glaze particles; mixing 40-80 parts of ceramic glaze particles and 60-100 parts of water, stirring at a temperature of 60-80° C. for 1-3 hours to obtain a mixed solution A; S2: Mix 3-6 parts of the first dispersant and 2-7 parts of the second dispersant, and stir at a temperature of 40-60° C. for 20-40 minutes to obtain a mixed dispersant; S3: Mix the mixed solution A described in step S1, the mixed dispersant described in step S2, 1-4 parts of stabilizer and 0.5-2 parts of anti-settling agent, perform ultrasonic treatment at a temperature of 35-45°C for 15-25 minutes, then add 2-4 parts of surfactant, and continue stirring for 25-45 minutes to obtain a water-based ceramic glaze ink.

[0009] Furthermore, the preparation of ceramic glaze particles in step S1 is specifically as follows: by weight, 1-4 parts of silicon dioxide, 2-5 parts of aluminum oxide, 1-3 parts of iron oxide, 2-5 parts of magnesium oxide, 1-3 parts of zinc oxide and 3-5 parts of barium oxide are mixed, calcined at a temperature of 1100-1200°C for 10-15 minutes, and ball-milled to a particle size of less than 10 μm.

[0010] Furthermore, the preparation process of the first dispersant in step S2 is as follows: by weight, 80-100 parts of epoxy phenolic resin, 20-40 parts of polyethylene glycol ether, 1-3 parts of boron trifluoride etherate, 20-40 parts of N,N-dimethylformamide and 3-6 parts of ethylene oxide are mixed, and stirred at a temperature of 80-100°C for 0.5-1.5h.

[0011] Furthermore, the preparation process of the second dispersant in step S2 is as follows: in parts by weight, 30-45 parts of vinyl butoxy polyoxyethylene ether, 10-20 parts of diethylene glycol monobutyl ether and 60-80 parts of deionized water are mixed, stirred at a temperature of 40-50°C for 30-50 minutes, then 1-3 parts of hydrogen peroxide and 0.5-1.5 parts of hypophosphorous acid are added, and stirring is continued for 10-20 minutes; then 5-10 parts of dodecyl tributyl ammonium bromide are added dropwise, and the reaction is kept warm at a temperature of 80-100°C for 35-45 minutes to obtain a second dispersant.

[0012] Furthermore, the preparation process of the stabilizer in step S3 is as follows: by weight, 20-40 parts of attapulgite are dispersed in deionized water, and the dispersion mass concentration is 10-20%; then 2-5 parts of a 10% mass fraction sodium hexametaphosphate aqueous solution, 1-3 parts of acrylamide monomer and 0.3-0.6 parts of ammonium persulfate are added, and the reaction is stirred at a temperature of 80-120° C. for 1.5-2.5 hours.

[0013] Furthermore, the preparation process of the anti-settling agent in step S3 is as follows: by weight, 10-20 parts of dimethyl adipate, 8-12 parts of decanol polyoxyethylene ether, 12-18 parts of sodium lauryl sulfate and 3-7 parts of propylene glycol are stirred and reacted at a temperature of 120-140° C. for 1-3 hours.

[0014] Furthermore, step S3 is further optimized as follows: mix the mixed liquid A described in step S1, the mixed dispersant described in step S2, 1-4 parts of stabilizer and 0.5-2 parts of anti-settling agent, ultrasonically treat for 18 minutes at a temperature of 40°C and a power of 2200W, then add 2-4 parts of surfactant, and continue stirring at a rate of 600r / min for 40 minutes to obtain a water-based ceramic glaze ink.

[0015] Compared with the prior art, the advantages and beneficial effects of the present invention are: 1. The present invention uses epoxy phenolic resin, polyethylene glycol ether, boron trifluoride ethyl ether, N,N-dimethylformamide and ethylene oxide as raw materials to prepare a first dispersant; uses vinyl butoxy polyoxyethylene ether, diethylene glycol monobutyl ether, hydrogen peroxide, hypophosphorous acid, dodecyl tributyl ammonium bromide and the like as raw materials to prepare a second dispersant; and forms a protective film to reduce the mutual attraction between particles, reduce the occurrence of agglomeration, increase the steric hindrance of the dispersant, and thus improve the dispersion efficiency.

[0016] 2. On the basis of the above, the present invention uses attapulgite loaded with sodium hexametaphosphate aqueous solution, acrylamide monomer, and ammonium persulfate to form a stabilizer; dimethyl adipate, decanol polyoxyethylene ether, sodium dodecyl sulfate and glycerol are used to form an anti-settling agent. Through the synergistic effect between the components, the prepared water-based ceramic glaze ink has excellent dispersion stability, surface tension and other properties. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0018] Example 1 This embodiment provides a method for preparing a water-based ceramic glaze ink with high stability, comprising the following steps: S1: 1g of silicon dioxide, 2g of aluminum oxide, 1g of iron oxide, 2g of magnesium oxide, 1g of zinc oxide and 3g of barium oxide were mixed, calcined at 1100°C for 10min, and ball-milled to a particle size of less than 10μm; 40g of ceramic glaze particles and 60g of water were mixed, and stirred at 60°C at a rate of 500r / min for 1h to obtain a mixed solution A; S2: 80g of epoxy phenolic resin, 20g of polyethylene glycol ether, 1g of boron trifluoride ether, 20g of N,N-dimethylformamide and 3g of ethylene oxide were mixed, and the mixture was stirred at 80°C and 600r / min for 0.5h to obtain a first dispersant; 30g of vinyl butoxy polyoxyethylene ether, 10g of diethylene glycol monobutyl ether and 60g of deionized water were mixed, and the mixture was stirred at 40°C and 600r / min for 30min, followed by adding 1g of hydrogen peroxide and 0.5g of hypophosphorous acid, and stirring was continued at 600r / min for 10-20min; 5g of dodecyltributylammonium bromide was then added dropwise, and the mixture was kept warm at 80°C for 35min to obtain a second dispersant; 3g of the first dispersant and 2g of the second dispersant were mixed, and the mixture was stirred at 40°C and 450r / min for 20min to obtain a mixed dispersant; S3: Disperse 20g of attapulgite in deionized water with a dispersion mass concentration of 10%; then add 2g of 10% sodium hexametaphosphate aqueous solution, 1g of acrylamide monomer and 0.3g of ammonium persulfate, stir and react at a temperature of 80°C and a rate of 300r / min for 1.5h to obtain a stabilizer; stir and react 10g of dimethyl adipate, 8g of decanol polyoxyethylene ether, 12g of sodium dodecyl sulfate and 3g of glycerol at a temperature of 120°C and a rate of 600 / min for 1h to obtain an anti-settling agent; The mixed solution A described in step S1, the mixed dispersant described in step S2, 1 g of stabilizer and 0.5 g of anti-settling agent were mixed, and ultrasonic treatment was performed at a temperature of 35° C. and a power of 2000 W for 15 min. Subsequently, 2 g of surfactant fatty alcohol polyoxyethylene ether was added, and stirring was continued at a rate of 800 / min for 25 min to obtain a water-based ceramic glaze ink.

[0019] Example 2 This embodiment provides a method for preparing a water-based ceramic glaze ink with high stability, comprising the following steps: S1: 4g of silicon dioxide, 5g of aluminum oxide, 3g of iron oxide, 5g of magnesium oxide, 3g of zinc oxide and 5g of barium oxide were mixed, calcined at 1200°C for 15min, and ball-milled to a particle size of less than 10μm; 80g of ceramic glaze particles and 100g of water were mixed, and stirred at 80°C at a rate of 500r / min for 3h to obtain a mixed solution A; S2: 100 g of epoxy phenolic resin, 40 g of polyethylene glycol ether, 3 g of boron trifluoride ether, 40 g of N,N-dimethylformamide and 6 g of ethylene oxide were mixed, and the mixture was stirred at 100°C at a rate of 400 r / min for 1.5 h to obtain a first dispersant; 45 g of vinyl butoxy polyoxyethylene ether, 20 g of diethylene glycol monobutyl ether and 80 g of deionized water were mixed, and the mixture was stirred at 50°C at a rate of 350 r / min for 50 min, followed by adding 3 g of hydrogen peroxide and 1.5 g of hypophosphorous acid, and stirring was continued at a rate of 400 r / min for 20 min; 10 g of dodecyl tributyl ammonium bromide was then added dropwise, and the mixture was kept warm at 100°C for 45 min to obtain a second dispersant; 6 g of the first dispersant and 7 g of the second dispersant were mixed, and the mixture was stirred at 60°C at a rate of 500 r / min for 40 min to obtain a mixed dispersant; S3: Disperse 40g of attapulgite in deionized water with a dispersion mass concentration of 10-20%; then add 5g of 10% sodium hexametaphosphate aqueous solution, 3g of acrylamide monomer and 0.6g of ammonium persulfate, stir and react at a temperature of 120°C and a speed of 600r / min for 2.5h to obtain a stabilizer; stir 20g of dimethyl adipate, 12g of decanol polyoxyethylene ether, 18g of sodium dodecyl sulfate and 7g of glycerol at a temperature of 140°C and a speed of 500r / min for 3h to obtain an anti-settling agent; The mixed solution A described in step S1, the mixed dispersant, 4 g of stabilizer and 2 g of anti-settling agent described in step S2 are mixed, and ultrasonic treatment is performed at a temperature of 45° C. and a power of 2500 W for 25 min. Then, 4 g of surfactant fatty alcohol polyoxyethylene ether is added, and stirring is continued at a speed of 500 r / min for 45 min to obtain a water-based ceramic glaze ink.

[0020] Example 3 This embodiment provides a method for preparing a water-based ceramic glaze ink with high stability, comprising the following steps: S1: 2.5 g of silicon dioxide, 3 g of aluminum oxide, 2 g of iron oxide, 4 g of magnesium oxide, 2 g of zinc oxide and 4 g of barium oxide were mixed, calcined at 1150°C for 12 min, and ball-milled to a particle size of less than 10 μm; 65 g of ceramic glaze particles and 85 g of water were mixed, and stirred at 75°C at a rate of 600 r / min for 2.5 h to obtain a mixed solution A; S2: 90g of epoxy phenolic resin, 35g of polyethylene glycol ether, 2g of boron trifluoride ether, 30g of N,N-dimethylformamide and 5g of ethylene oxide were mixed, and the mixture was stirred at 90°C at a rate of 500r / min for 1.2h to obtain a first dispersant; 40g of vinyl butoxy polyoxyethylene ether, 15g of diethylene glycol monobutyl ether and 70g of deionized water were mixed, and the mixture was stirred at 45°C at a rate of 500r / min for 45min, followed by adding 2g of hydrogen peroxide and 1g of hypophosphorous acid, and stirring was continued at a rate of 350r / min for 15min; 7g of dodecyltributylammonium bromide was then added dropwise, and the mixture was kept warm at 90°C for 40min to obtain a second dispersant; 5g of the first dispersant and 4g of the second dispersant were mixed, and the mixture was stirred at 55°C at a rate of 400r / min for 25min to obtain a mixed dispersant; S3: Disperse 35g of attapulgite in deionized water with a dispersion mass concentration of 13%; then add 3g of 10% sodium hexametaphosphate aqueous solution, 2g of acrylamide monomer and 0.4g of ammonium persulfate, stir and react at a temperature of 100°C and a speed of 450r / min for 2h to obtain a stabilizer; stir and react 16g of dimethyl adipate, 10g of decanol polyoxyethylene ether, 15g of sodium dodecyl sulfate and 5g of glycerol at a temperature of 130°C and a speed of 600r / min for 2h to obtain an anti-settling agent; The mixed solution A described in step S1, the mixed dispersant described in step S2, 2.5 g of stabilizer and 1.5 g of anti-settling agent were mixed, and ultrasonic treatment was performed at 2500 W for 22 min at a temperature of 42° C., and then 3 g of surfactant fatty alcohol polyoxyethylene ether was added, and stirring was continued at a rate of 400 r / min for 36 min to obtain a water-based ceramic glaze ink.

[0021] Comparative Example 1 The difference between this comparative example and Example 1 is that the ceramic glaze particles prepared in step S1 do not contain iron oxide, magnesium oxide, and zinc oxide, and the other steps are the same.

[0022] Comparative Example 2 The difference between this comparative example and Example 1 is that the first dispersant is not added in step S2, and the other steps are the same.

[0023] Comparative Example 3 The difference between this comparative example and Example 1 is that the second dispersant is not added in step S2, and the other steps are the same.

[0024] Comparative Example 4 The difference between this comparative example and Example 1 is that no stabilizer is added in step S3, and the other steps are the same.

[0025] Comparative Example 5 The difference between this comparative example and Example 1 is that no anti-settling agent is added in step S3, and the other steps are the same.

[0026] Comparative Example 6 The difference between this comparative example and Example 1 is that no surfactant is added in step S3, and the other steps are the same.

[0027] Performance Test: Refer to GB / T 10247-2008 for testing viscosity, GB-T 22237-2008 for testing surface tension, and GB / T 6288-2021 for testing particle size; place in a 60℃ oven for 20 days, test the precipitation rate, precipitation rate = precipitation mass / total solution mass; print fluency, use the printer to print ink, and according to the printing effect, the atmosphere is good, good, average, and poor. The results are shown in the table below: Table 1 Performance test results

[0028] From the above performance test results, it can be seen that Examples 1-3 have good viscosity, dispersant, particle size, stability and printing fluency. In particular, the comprehensive performance of Example 3 is the most outstanding. However, since the comparative example does not adopt the necessary technical solution, it is significantly worse than the example in the corresponding performance test. The above experimental results further prove the importance of the technical solution defined in the present invention for its technical effect.

[0029] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A highly stable water-based ceramic glaze ink, characterized in that: The invention comprises the following components in parts by weight: 40-80 parts of ceramic glaze particles, 3-6 parts of a first dispersant, 2-7 parts of a second dispersant, 1-4 parts of a stabilizer, 0.5-2 parts of an anti-settling agent, 2-4 parts of a surfactant and 60-100 parts of water.

2. The highly stable aqueous ceramic glaze ink according to claim 1, characterized in that: The composition includes the following components in parts by weight: 65 parts of ceramic glaze particles, 5 parts of a first dispersant, 4.5 parts of a second dispersant, 2.5 parts of a stabilizer, 1 part of an anti-settling agent, 3 parts of a surfactant, and 85 parts of water.

3. The highly stable aqueous ceramic glaze ink according to claim 1, characterized in that: The surfactant is fatty alcohol polyoxyethylene ether.

4. A method for preparing a highly stable aqueous ceramic glaze ink, characterized in that: The steps include: S1: preparing ceramic glaze particles; mixing 40-80 parts of ceramic glaze particles and 60-100 parts of water, stirring at a temperature of 60-80° C. for 1-3 hours to obtain a mixed solution A; S2: Mix 3-6 parts of the first dispersant and 2-7 parts of the second dispersant, and stir at a temperature of 40-60° C. for 20-40 minutes to obtain a mixed dispersant; S3: Mix the mixed solution A described in step S1, the mixed dispersant described in step S2, 1-4 parts of stabilizer and 0.5-2 parts of anti-settling agent, perform ultrasonic treatment at a temperature of 35-45°C for 15-25 minutes, then add 2-4 parts of surfactant, and continue stirring for 25-45 minutes to obtain a water-based ceramic glaze ink.

5. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: The preparation of ceramic glaze particles in step S1 is specifically as follows: by weight, 1-4 parts of silicon dioxide, 2-5 parts of aluminum oxide, 1-3 parts of iron oxide, 2-5 parts of magnesium oxide, 1-3 parts of zinc oxide and 3-5 parts of barium oxide are mixed, calcined at a temperature of 1100-1200° C. for 10-15 minutes, and ball-milled to a particle size of less than 10 μm.

6. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: The preparation process of the first dispersant in step S2 is as follows: by weight, 80-100 parts of epoxy phenolic resin, 20-40 parts of polyethylene glycol ether, 1-3 parts of boron trifluoride etherate, 20-40 parts of N,N-dimethylformamide and 3-6 parts of ethylene oxide are mixed, and stirred at a temperature of 80-100° C. for reaction for 0.5-1.5 hours.

7. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: The preparation process of the second dispersant in step S2 is as follows: In parts by weight, 30-45 parts of vinyl butoxy polyoxyethylene ether, 10-20 parts of diethylene glycol monobutyl ether and 60-80 parts of deionized water are mixed, stirred at a temperature of 40-50° C. for 30-50 minutes, then 1-3 parts of hydrogen peroxide and 0.5-1.5 parts of hypophosphorous acid are added, and stirring is continued for 10-20 minutes; Then 5-10 parts of dodecyltributylammonium bromide are added dropwise, and the mixture is kept at 80-100°C for 35-45 minutes to obtain a second dispersant.

8. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: The preparation process of the stabilizer in step S3 is as follows: by weight, 20-40 parts of attapulgite are dispersed in deionized water, and the dispersion mass concentration is 10-20%; then 2-5 parts of a 10% by weight aqueous solution of sodium hexametaphosphate, 1-3 parts of acrylamide monomer and 0.3-0.6 parts of ammonium persulfate are added, and the reaction is stirred at a temperature of 80-120° C. for 1.5-2.5 hours.

9. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: The preparation process of the anti-settling agent in step S3 is as follows: by weight, 10-20 parts of dimethyl adipate, 8-12 parts of decanol polyoxyethylene ether, 12-18 parts of sodium lauryl sulfate and 3-7 parts of propylene glycol are stirred and reacted at a temperature of 120-140° C. for 1-3 hours.

10. The method for preparing a highly stable aqueous ceramic glaze ink according to claim 3, characterized in that: Step S3 is further optimized as follows: the mixed solution A described in step S1, the mixed dispersant described in step S2, 1-4 parts of the stabilizer and 0.5-2 parts of the anti-settling agent are mixed, ultrasonically treated at a temperature of 40°C and a power of 2200W for 18 minutes, and then 2-4 parts of the surfactant are added, and stirring is continued at a rate of 600r / min for 40 minutes to obtain a water-based ceramic glaze ink.

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