Ceramic dry granulation molding plasticizer

Abstract

The invention discloses a ceramic dry granulation forming plasticizer in the field of ceramic material production. The plasticizer comprises the following raw materials: a paraffin base material, rosin emulsion accounting for 3-6wt% of the mass of the paraffin base material, stearic acid accounting for 1-3wt% of the mass of the paraffin base material, and a flow promoter accounting for 2-4wt% of the mass of the paraffin base material. Wherein the flow promoter is formed by compounding lacquer fruit wax and an oroxylum indicum seed extract according to the mass ratio of 1: 10. According to the plasticizer, paraffin is used as a base material, rosin emulsion is added to improve chemical stability, stearic acid is added to improve dispersion and fusion effects, and a flow promoter composed of oroxylum indicum seed extract and lacquer fruit wax in a specific proportion is added, so that a thin smooth film can be formed on the surfaces of particles, the friction coefficient between the particles is reduced, and the fluidity of the particles is improved; in addition, the viscosity of the oroxylum indicum seed extract is adjusted by using the hydrophobicity and lubricity of the lacquer fruit wax, so that the oroxylum indicum seed extract provides a proper bonding effect, the particle forming quality is enhanced, and the ratio of effective particles in the granulation powder is increased.

Description

Technical Field

[0001] The invention relates to the technical field of ceramic material production, in particular to a ceramic dry granulation molding plasticizer. Background Art

[0002] The traditional processing method for ceramic granular powder is wet granulation, which mainly involves wet ball milling. Then, the slurry with a moisture content of approximately 35-38% is spray-dried to obtain a powder with a moisture content of 6-7%. The powder is then pressed to form granules. In the wet granulation mode, spray granulation of the slurry with a high moisture content requires a large amount of heat energy and consumes a lot of energy. To solve this energy consumption problem, more research is currently focusing on dry granulation. Compared with wet granulation, dry granulation has lower energy consumption and higher efficiency, making it a major measure for ceramic manufacturers to reduce costs, energy consumption, and emissions.

[0003] During the dry granulation process, a dry granulator applies high pressure (usually 10-50 MPa) to the mixed powder to form granules. Under the action of high pressure, the powder particles are combined by van der Waals forces, mechanical bite, etc. This combination method has high requirements for the plasticity and fluidity of the powder. Therefore, a certain amount of plasticizer can be added during the granulation process. The expected role of the plasticizer is to: (1) Improve plasticity: reduce the friction between powder particles, enhance the deformation ability of powder under high pressure, promote particle bonding, improve the quality of particle molding, and increase the proportion of effective particles. (2) Improve fluidity: reduce powder agglomeration, improve the fluidity and filling properties of particles, and facilitate subsequent molding processes. (3) Reduce equipment wear: The lubricating effect reduces the friction between the powder and the granulator mold, extending the life of the equipment.

[0004] However, there are relatively few types of plasticizers currently used in ceramic dry granulation molding processes, and they are generally single components, such as polyvinyl alcohol and paraffin. These plasticizers are not very effective in increasing the proportion of effective particles and improving fluidity. Summary of the Invention

[0005] The object of the present invention is to provide a ceramic dry granulation molding plasticizer, which solves the problem that the existing plasticizers used in the ceramic dry granulation molding process are not effective in increasing the proportion of effective particles and improving fluidity.

[0006] The present invention achieves the above-mentioned purpose through the following technical solutions:

[0007] A ceramic dry granulation molding plasticizer, the raw materials of the plasticizer include a paraffin base material, 3-6wt% of rosin emulsion, 1-3wt% of stearic acid, and 2-4wt% of a flow promoter;

[0008] The flow promoter is composed of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:10.

[0009] A further improvement is that the raw materials of the plasticizer include paraffin base material, 5 wt% of rosin emulsion, 2 wt% of stearic acid, and 3 wt% of flow promoter based on the mass of the paraffin base material.

[0010] A further improvement is that the rosin emulsion is prepared by heating the masson pine rosin to 112-116° C. to melt the mixture and then mixing it with an emulsifier ONISTAPS-350; stirring the mixture at 400-600 rpm for 25-30 minutes; cooling the mixture to 98-102° C. and then adding boiling water dropwise; continuing to stir and react for 8-12 minutes; cooling the reaction solution to room temperature; and filtering the filtrate to obtain the rosin emulsion.

[0011] A further improvement is that the mass ratio of the masson pine rosin, the emulsifier ONISTAPS-350 and the boiling water is 10:4-5:20-25.

[0012] A further improvement is that the preparation steps of the Oroxylum indica seed extract are:

[0013] S1. Seed pretreatment and extraction

[0014] Oroxylum butterfly seeds were crushed and sieved to separate the seed kernels from the winglets to obtain Oroxylum butterfly seed kernel powder with a particle size of 0.5-1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:8-10, and the mixture was heated and refluxed for extraction. The mixture was then filtered and concentrated under reduced pressure of -0.08 to -0.1 MPa to obtain a crude extract.

[0015] S2. Elution and purification

[0016] Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 24-36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 1.5-2.5 BV / h until the effluent is colorless and transparent. Then use deionized water to elute at the same flow rate until the effluent has no alcohol smell.

[0017] Load the crude extract onto the resin column at a flow rate of 0.8-1 mL / min. After loading, close the column valve and let it stand for 12-18 hours.

[0018] First, water-soluble impurities are eluted with deionized water until the eluate is clear, and then 4-6 BV of ethanol aqueous solution with a volume concentration of 30% is added to elute, the eluate is discarded, and then 4-6 BV of ethanol aqueous solution with a volume concentration of 60% is added to elute, the eluate of this part is collected, and it is concentrated under reduced pressure at -0.08 to -0.1 MPa until there is no alcohol taste, and finally freeze-dried to obtain the Oroxylum butterfly seed extract.

[0019] A further improvement is that the heating reflux extraction refers to controlling the temperature to 78-82°C for heating reflux extraction, and the extraction time is 2-3 hours, and a total of 2-3 extractions.

[0020] A further improvement is that the flow rates when eluting with deionized water and ethanol aqueous solution are both 1.5-2.5 BV / h.

[0021] A further improvement is that the freeze-drying temperature is -40°C, the pressure is 5-10 Pa, and the time is 24-48 hours.

[0022] A further improvement is that the plasticizer is obtained by heating a paraffin base to 75-85° C. to melt it, then mixing rosin emulsion, stearic acid, oroxylum seed extract and lacquer fruit wax into it and stirring evenly, and then standing to cool.

[0023] The beneficial effects of the present invention are as follows: the plasticizer of the present invention uses paraffin as a base material, adds rosin emulsion to improve chemical stability, adds stearic acid to improve dispersion and fusion effects, and adds a flow promoter composed of a specific proportion of oroxylum butterfly seed extract and lacquer fruit wax, which can form a thin smooth film on the surface of the particles, reduce the friction coefficient between the particles, and improve the fluidity of the particles. In addition, the hydrophobicity and lubricity of the lacquer fruit wax are utilized to adjust the viscosity of the oroxylum butterfly seed extract, so that it provides a moderate bonding effect, enhances the particle molding quality, and increases the proportion of effective particles in the granulated powder. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 Schematic diagram of the particle size distribution of each group of granulating powder in the effective particle test. DETAILED DESCRIPTION

[0025] The present application is described in further detail below in conjunction with the accompanying drawings. It is necessary to point out that the following specific implementation methods are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Technicians in this field can make some non-essential improvements and adjustments to the present application based on the above application content.

[0026] 1. Main Materials

[0027] Industrial paraffin: purchased from Guangzhou Fufei Chemical Technology Co., Ltd.

[0028] Masson pine rosin: purchased from Jiangxi Fuda Flavor Chemical Co., Ltd.

[0029] Stearic acid: purchased from Guangzhou Zhongyi Chemical Co., Ltd.

[0030] Oroxylum seeds: purchased from Bozhou medicinal material market in Anhui Province;

[0031] Lacquer wax: purchased from Shanghai Peihong New Materials Technology Co., Ltd.

[0032] 2. Implementation of the Experiment

[0033] Example 1

[0034] A plasticizer for ceramic dry granulation molding, comprising a paraffin base, 3% by weight of rosin emulsion, 1% by weight of stearic acid, and 2% by weight of a flow promoter; the flow promoter is a mixture of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:10. The plasticizer is prepared by heating the paraffin base to 75°C to melt it, then mixing the rosin emulsion, stearic acid, oroxylum butterfly seed extract, and lacquer fruit wax, stirring uniformly, and allowing the mixture to cool.

[0035] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 112° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 400 rpm for 30 minutes, cooling the mixture to 98° C. and then adding boiling water dropwise, continuing to stir and react for 12 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:4:20.

[0036] The preparation steps of Oroxylum indica seed extract are as follows:

[0037] S1. Seed pretreatment and extraction

[0038] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 0.5 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:8, and the mixture was heated and refluxed at 78°C for 2 hours. The extraction was performed twice, and the mixture was then filtered and concentrated under reduced pressure of -0.08 MPa to obtain a crude extract.

[0039] S2. Elution and purification

[0040] Take D101 macroporous resin, soak it in 95% ethanol aqueous solution by volume for 24 hours, and then wet-pack it into a column. The resin column bed volume (BV) is controlled to 300 mL. After packing, pass 95% ethanol aqueous solution by volume at a flow rate of 1.5 BV / h until the effluent is colorless and transparent. Then use deionized water to elute at the same flow rate until the effluent has no alcohol smell.

[0041] The crude extract was loaded onto the resin column at a flow rate of 0.8 mL / min. After loading, the column valve was closed and the column was allowed to stand for 12 h.

[0042] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 4 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 4 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.08 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 5 Pa, time 24 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 1.5 BV / h.

[0043] Example 2

[0044] A plasticizer for ceramic dry granulation molding, comprising a paraffin base, 5% by weight of rosin emulsion, 2% by weight of stearic acid, and 3% by weight of a flow promoter; the flow promoter is a mixture of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:10. The plasticizer is prepared by heating the paraffin base to 80°C to melt it, then mixing the rosin emulsion, stearic acid, oroxylum butterfly seed extract, and lacquer fruit wax, stirring uniformly, and allowing the mixture to cool.

[0045] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 114° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting it at a speed of 500 rpm for 28 minutes, cooling it to 100° C. and then adding boiling water dropwise, continuing to stir and react for 10 minutes, cooling the obtained reaction solution to room temperature, and filtering to obtain the filtrate. The mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:4.5:22.

[0046] The preparation steps of Oroxylum indica seed extract are as follows:

[0047] S1. Seed pretreatment and extraction

[0048] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 0.8 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:9. The extraction was carried out by heating and refluxing at 80°C for 2 hours. The extraction was repeated 3 times, and then the crude extract was filtered and concentrated under reduced pressure of -0.1 MPa to obtain a crude extract.

[0049] S2. Elution and purification

[0050] Take D101 macroporous resin, soak it in 95% ethanol aqueous solution by volume for 30 hours, and then wet-pack it into a column. The resin column bed volume (BV) is controlled to 300 mL. After packing, pass 95% ethanol aqueous solution by volume at a flow rate of 2 BV / h until the effluent is colorless and transparent. Then use deionized water to elute at the same flow rate until the effluent has no alcohol smell.

[0051] The crude extract was loaded onto the resin column at a flow rate of 1 mL / min. After loading, the column valve was closed and the column was allowed to stand for 15 h.

[0052] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 5 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 5 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.1 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 8 Pa, time 36 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 2 BV / h.

[0053] Example 3

[0054] A plasticizer for ceramic dry granulation molding, comprising a paraffin base, 6% by weight of rosin emulsion, 3% by weight of stearic acid, and 4% by weight of a flow promoter; the flow promoter is a mixture of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:10. The plasticizer is prepared by heating the paraffin base to 85°C to melt it, then mixing the rosin emulsion, stearic acid, oroxylum butterfly seed extract, and lacquer fruit wax, stirring uniformly, and allowing the mixture to cool.

[0055] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 116° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 600 rpm for 25 minutes, cooling the mixture to 102° C. and then adding boiling water dropwise, continuing to stir and react for 8 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:5:25.

[0056] The preparation steps of Oroxylum indica seed extract are as follows:

[0057] S1. Seed pretreatment and extraction

[0058] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:10, and the mixture was heated and refluxed at 82°C for 3 hours. The extraction was repeated 3 times, and then the crude extract was filtered and concentrated under reduced pressure of -0.1 MPa to obtain a crude extract.

[0059] S2. Elution and purification

[0060] Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 2.5 BV / h until the effluent is colorless and transparent. Then use deionized water at the same flow rate to elute until the effluent has no alcohol smell.

[0061] The crude extract was loaded onto the resin column at a flow rate of 1 mL / min. After loading, the column valve was closed and allowed to stand for 18 h.

[0062] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 6 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 6 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.1 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 10 Pa, time 48 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 2.5 BV / h.

[0063] Comparative Example 1

[0064] A plasticizer for ceramic dry granulation molding, comprising a paraffin base, 6% by weight of rosin emulsion, 3% by weight of stearic acid, and 4% by weight of a flow promoter; the flow promoter is a mixture of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:5. The plasticizer is prepared by heating the paraffin base to 85°C to melt it, then mixing the rosin emulsion, stearic acid, oroxylum butterfly seed extract, and lacquer fruit wax, stirring uniformly, and allowing the mixture to cool.

[0065] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 116° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 600 rpm for 25 minutes, cooling the mixture to 102° C. and then adding boiling water dropwise, continuing to stir and react for 8 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:5:25.

[0066] The preparation steps of Oroxylum indica seed extract are as follows:

[0067] S1. Seed pretreatment and extraction

[0068] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:10, and the mixture was heated and refluxed at 82°C for 3 hours. The extraction was repeated 3 times, and then the crude extract was filtered and concentrated under reduced pressure of -0.1 MPa to obtain a crude extract.

[0069] S2. Elution and purification

[0070] Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 2.5 BV / h until the effluent is colorless and transparent. Then use deionized water at the same flow rate to elute until the effluent has no alcohol smell.

[0071] The crude extract was loaded onto the resin column at a flow rate of 1 mL / min. After loading, the column valve was closed and allowed to stand for 18 h.

[0072] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 6 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 6 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.1 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 10 Pa, time 48 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 2.5 BV / h.

[0073] Comparative Example 2

[0074] A plasticizer for ceramic dry granulation molding is disclosed. The plasticizer comprises a paraffin base, 6% by weight of a rosin emulsion, 3% by weight of stearic acid, and 4% by weight of a flow promoter. The flow promoter is a mixture of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:20. The plasticizer is prepared by heating the paraffin base to 85°C to melt it, then mixing the rosin emulsion, stearic acid, oroxylum butterfly seed extract, and lacquer fruit wax, stirring uniformly, and allowing the mixture to cool.

[0075] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 116° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 600 rpm for 25 minutes, cooling the mixture to 102° C. and then adding boiling water dropwise, continuing to stir and react for 8 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:5:25.

[0076] The preparation steps of Oroxylum indica seed extract are as follows:

[0077] S1. Seed pretreatment and extraction

[0078] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:10, and the mixture was heated and refluxed at 82°C for 3 hours. The extraction was repeated 3 times, and then the crude extract was filtered and concentrated under reduced pressure of -0.1 MPa to obtain a crude extract.

[0079] S2. Elution and purification

[0080] Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 2.5 BV / h until the effluent is colorless and transparent. Then use deionized water at the same flow rate to elute until the effluent has no alcohol smell.

[0081] The crude extract was loaded onto the resin column at a flow rate of 1 mL / min. After loading, the column valve was closed and allowed to stand for 18 h.

[0082] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 6 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 6 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.1 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 10 Pa, time 48 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 2.5 BV / h.

[0083] Comparative Example 3

[0084] A ceramic dry granulation molding plasticizer comprises raw materials including a paraffin base material, 6 wt% of rosin emulsion, 3 wt% of stearic acid, and 4 wt% of a flow promoter; the flow promoter is a single component of oroxylum butterfly seed extract. The plasticizer is prepared by heating the paraffin base material to 85°C to melt it, then mixing the rosin emulsion, stearic acid, and oroxylum butterfly seed extract into the mixture, stirring the mixture evenly, and allowing the mixture to cool.

[0085] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 116° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 600 rpm for 25 minutes, cooling the mixture to 102° C. and then adding boiling water dropwise, continuing to stir and react for 8 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:5:25.

[0086] The preparation steps of Oroxylum indicum seed extract are as follows:

[0087] S1. Seed pretreatment and extraction

[0088] The seeds of Oroxylum butterfly were crushed and sieved to separate the seed kernels from the wings to obtain Oroxylum butterfly seed kernel powder with a particle size of about 1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:10, and the mixture was heated and refluxed at 82°C for 3 hours. The extraction was repeated 3 times, and then the crude extract was filtered and concentrated under reduced pressure of -0.1 MPa to obtain a crude extract.

[0089] S2. Elution and purification

[0090] Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 2.5 BV / h until the effluent is colorless and transparent. Then use deionized water at the same flow rate to elute until the effluent has no alcohol smell.

[0091] The crude extract was loaded onto the resin column at a flow rate of 1 mL / min. After loading, the column valve was closed and allowed to stand for 18 h.

[0092] First, water-soluble impurities were eluted with deionized water until the eluate was clear. Then, 6 BV of ethanol solution with a volume concentration of 30% was added to elute. The eluate was discarded and 6 BV of ethanol solution with a volume concentration of 60% was added to elute. The eluate from this part was collected and concentrated under reduced pressure at -0.1 MPa until there was no alcohol smell. Finally, it was freeze-dried (temperature -40°C, pressure 10 Pa, time 48 hours) to obtain the Oroxylum indica seed extract. The flow rate for elution with deionized water and ethanol solution was 2.5 BV / h.

[0093] Comparative Example 4

[0094] A plasticizer for ceramic dry granulation molding is described. The plasticizer's raw materials include a paraffin base, 6% by weight of rosin emulsion, 3% by weight of stearic acid, and 4% by weight of a flow promoter. The flow promoter is a single component of lacquer fruit wax. The plasticizer is prepared by heating the paraffin base to 85°C to melt it, then mixing the rosin emulsion, stearic acid, and lacquer fruit wax, stirring evenly, and then allowing the mixture to cool.

[0095] The preparation steps of the rosin emulsion are as follows: heating Masson pine rosin to 116° C. to melt the mixture and then mixing it with emulsifier ONISTAPS-350, stirring and reacting at a speed of 600 rpm for 25 minutes, cooling the mixture to 102° C. and then adding boiling water dropwise, continuing to stir and react for 8 minutes, cooling the reaction solution to room temperature, and filtering to obtain the filtrate, wherein the mass ratio of the Masson pine rosin, emulsifier ONISTAPS-350 and boiling water is 10:5:25.

[0096] 3. Performance Testing

[0097] The raw materials used for dry granulation (purchased from Guangdong Mona Lisa New Building Materials Co., Ltd.) have a chemical composition as shown in Table 1 below:

[0098] Table 1: Chemical composition of dry granulation raw materials

[0099]

[0100] The above raw materials were subjected to dry grinding to obtain micropowders with an average particle size of about 12 μm. The plasticizers prepared in the above Examples 1-3 and Comparative Examples 1-4 were then heated to 100° C. to melt them. The plasticizers of each group were then mixed with the micropowders at a mass ratio of 1:50 of plasticizer to micropowder. After thorough stirring and mixing, the mixtures were granulated using a dry granulator (purchased from Yantai Hongke New Materials Co., Ltd.) to obtain granulated powders of each group. A blank group (granulated powders without any plasticizer) was also set up. The granulated powders of each group were subjected to the following performance tests:

[0101] (1) Effective particle test

[0102] The granulated powders obtained above were taken from each group and subjected to conventional drying treatment. The particle size distribution of each group of granulated powders was then tested by a screening method, that is, a multi-stage vibrating particle screening machine was used to screen out granulated powders of 20 mesh, 30 mesh, 40 mesh, 50 mesh, 60 mesh, 70 mesh and 80 mesh, respectively. Then, a high-precision electronic balance was used to weigh them in sequence, and the mass percentages of granulated powders with particle sizes greater than 20 mesh, 20-30 mesh, 30-40 mesh, 40-50 mesh, 50-60 mesh, 60-70 mesh, 70-80 mesh and less than 80 mesh were calculated, respectively. The granulated powder with a particle size of 20-80 mesh was taken as the effective particles, and the proportion of effective particles in each group was counted.

[0103] (2) Liquidity test

[0104] The BT-1000 powder comprehensive property tester produced by Liaoning Dandong Better Company was used to measure the angle of repose, flat angle, compression degree and uniformity of each group of granulated powders obtained above. Then, the flowability index of each group of granulated powders was calculated with the help of the Carr flowability index method to analyze the flowability of the granulated powders.

[0105] 4. Results Analysis

[0106] (1) Effective particle test

[0107] Table 2: Results of effective particle ratio of granulation powder in each group

[0108]

[0109]

[0110] After testing, the particle size distribution of each group of granulated powder is as follows Figure 1 As shown, the effective particle ratio data are shown in Table 2 above. It can be seen that the plasticizers prepared in Examples 1-3 of the present invention can significantly improve the particle molding quality of the granulated powder, and the effective particle ratio is increased from 58.4% to more than 85.4% compared with the blank group, especially in Example 2, where the effective particle ratio reaches 90.1%, and the specific particle size distribution is also more concentrated in the range of 40-60 mesh. Comparative Examples 1-4 are all adjustments made on the basis of Example 3, wherein: Comparative Examples 1 and 2 adjust the mass ratio of lacquer fruit wax and oroxylum butterfly seed extract in the flow promoter to 1:5 and 1:20, respectively, so that the effective particle ratio is reduced to 80.2% and 79.4%, respectively. In Comparative Examples 3 and 4, the flow promoter only uses a single component of oroxylum butterfly seed extract or lacquer fruit wax, respectively, so that the effective particle ratio is reduced to 76.2% and 73.6%, respectively.

[0111] (2) Liquidity test

[0112] Table 3: Flowability index of granulated powders in each group

[0113]

[0114] After testing, the fluidity index of each group of granulated powder is shown in Table 3 above. It can be seen that the plasticizers prepared in Examples 1-3 of the present invention can significantly improve the fluidity of the granulated powder, and the fluidity index is increased from 61 to more than 83 compared with the blank group, especially in Example 2, the fluidity index is even 88. Similarly, the adjustments made in Comparative Examples 1-4 on the basis of Example 3 are as follows: Comparative Examples 1 and 2 adjust the mass ratio of lacquer fruit wax to oroxylum butterfly seed extract in the flow promoter to 1:5 and 1:20, respectively, so that the fluidity index decreases to 76.5 and 72, respectively. In Comparative Examples 3 and 4, the flow promoter uses only oroxylum butterfly seed extract or lacquer fruit wax as a single component, respectively, so that the proportion of effective particles decreases to 64.5 and 71, respectively.

[0115] Based on the above analysis, the plasticizer prepared by the present invention has an outstanding application effect in ceramic dry granulation, can improve the fluidity of the particles, and increase the proportion of effective particles in the granulated powder, which is very important for the later ceramic body forming and sintering process. In addition, the ratio of the orchid butterfly seed extract and the lacquer fruit wax in the flow promoter used also needs to be controlled. Existing experiments show that the effect is best when the lacquer fruit wax and the orchid butterfly seed extract are compounded in a mass ratio of 1:10, which can achieve a synergistic effect. Adding too much or too little lacquer fruit wax will lead to a deterioration of the effect, and adding only one component of lacquer fruit wax or orchid butterfly seed extract will have a worse effect.

[0116] The above-described embodiments merely illustrate several implementations of the present invention. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, and all such variations and improvements fall within the scope of protection of the present invention.

Claims

1. A ceramic dry granulation molding plasticizer, characterized in that: The raw materials of the plasticizer include paraffin base material, rosin emulsion accounting for 3-6wt% of the mass of the paraffin base material, stearic acid accounting for 1-3wt% and flow promoter accounting for 2-4wt%; The flow promoter is composed of lacquer fruit wax and oroxylum butterfly seed extract in a mass ratio of 1:

10.

2. A ceramic dry granulation molding plasticizer according to claim 1, characterized in that, The raw materials of the plasticizer include paraffin base material, rosin emulsion accounting for 5wt% of the mass of the paraffin base material, stearic acid accounting for 2wt% and flow promoter accounting for 3wt%.

3. A ceramic dry granulation molding plasticizer according to claim 1, characterized in that: The rosin emulsion is prepared by heating Masson pine rosin to 112-116° C. to melt the mixture and then mixing it with an emulsifier ONISTAPS-350; stirring the mixture at 400-600 rpm for 25-30 minutes; cooling the mixture to 98-102° C. to dropwise add boiling water; continuing stirring the mixture for 8-12 minutes; cooling the reaction solution to room temperature; and filtering the filtrate to obtain the rosin emulsion.

4. A ceramic dry granulation molding plasticizer according to claim 3, characterized in that: The mass ratio of the masson pine rosin, the emulsifier ONISTAPS-350 and the boiling water is 10:4-5:20-25.

5. A ceramic dry granulation molding plasticizer according to claim 1, characterized in that: The preparation steps of the Oroxylum indica seed extract are as follows: S1. Seed pretreatment and extraction Oroxylum butterfly seeds were crushed and sieved to separate the seed kernels from the winglets to obtain Oroxylum butterfly seed kernel powder with a particle size of 0.5-1 mm. A 60% ethanol aqueous solution was added at a solid-liquid ratio of 1:8-10, and the mixture was heated and refluxed for extraction. The mixture was then filtered and concentrated under reduced pressure of -0.08 to -0.1 MPa to obtain a crude extract. S2. Elution and purification Take D101 macroporous resin and soak it in 95% ethanol aqueous solution for 24-36 hours. Then wet-pack it into a column with a resin bed volume (BV) of 300 mL. After packing, pass 95% ethanol aqueous solution at a flow rate of 1.5-2.5 BV / h until the effluent is colorless and transparent. Then use deionized water to elute at the same flow rate until the effluent has no alcohol smell. Load the crude extract onto the resin column at a flow rate of 0.8-1 mL / min. After loading, close the column valve and let it stand for 12-18 hours. First, water-soluble impurities are eluted with deionized water until the eluate is clear, and then 4-6 BV of ethanol aqueous solution with a volume concentration of 30% is added to elute, the eluate is discarded, and then 4-6 BV of ethanol aqueous solution with a volume concentration of 60% is added to elute, the eluate of this part is collected, and it is concentrated under reduced pressure at -0.08 to -0.1 MPa until there is no alcohol taste, and finally freeze-dried to obtain the Oroxylum butterfly seed extract.

6. A ceramic dry granulation molding plasticizer according to claim 5, characterized in that: The heating reflux extraction refers to controlling the temperature to be 78-82° C. for heating reflux extraction, and the extraction time is 2-3 hours, and the extraction is performed 2-3 times in total.

7. A ceramic dry granulation molding plasticizer according to claim 5, characterized in that: The flow rates for elution with deionized water and ethanol aqueous solution were both 1.5-2.5 BV / h.

8. A ceramic dry granulation molding plasticizer according to claim 5, characterized in that: The freeze-drying temperature is -40°C, the pressure is 5-10 Pa, and the time is 24-48 hours.

9. A ceramic dry granulation molding plasticizer according to any one of claims 1 to 8, characterized in that: The plasticizer is obtained by heating a paraffin base material to 75-85 DEG C to melt it, then mixing rosin emulsion, stearic acid, oroxylum seed extract and lacquer fruit wax into the mixture, stirring the mixture evenly, and then standing the mixture to cool.

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