CN111763090B - Adhesive, preparation method and application thereof - Google Patents
Adhesive, preparation method and application thereof Download PDFInfo
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- CN111763090B CN111763090B CN202010480350.8A CN202010480350A CN111763090B CN 111763090 B CN111763090 B CN 111763090B CN 202010480350 A CN202010480350 A CN 202010480350A CN 111763090 B CN111763090 B CN 111763090B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000853 adhesive Substances 0.000 title claims description 9
- 230000001070 adhesive effect Effects 0.000 title claims description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 52
- 239000000919 ceramic Substances 0.000 claims abstract description 51
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 41
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000002347 injection Methods 0.000 claims abstract description 38
- 239000007924 injection Substances 0.000 claims abstract description 38
- 238000001746 injection moulding Methods 0.000 claims abstract description 32
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims abstract description 5
- 238000000197 pyrolysis Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 48
- 239000002245 particle Substances 0.000 claims description 37
- 238000007599 discharging Methods 0.000 claims description 35
- 239000003292 glue Substances 0.000 claims description 34
- 238000001816 cooling Methods 0.000 claims description 18
- 238000000354 decomposition reaction Methods 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 17
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 16
- 239000001993 wax Substances 0.000 claims description 13
- 238000004898 kneading Methods 0.000 claims description 12
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 8
- 229920002125 Sokalan® Polymers 0.000 claims description 8
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 8
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000004584 polyacrylic acid Substances 0.000 claims description 8
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- 235000019808 microcrystalline wax Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 125000000129 anionic group Chemical group 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
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- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000012188 paraffin wax Substances 0.000 claims description 4
- 235000013871 bee wax Nutrition 0.000 claims description 3
- 239000012166 beeswax Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 description 16
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
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- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
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- 238000004260 weight control Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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Abstract
The invention discloses a binder and a preparation method and application thereof, wherein the binder comprises the following components in parts by weight: 3-10 parts of low molecular weight wax component, 20-50 parts of 1# polyacrylic resin, 0-30 parts of 2# polyacrylic resin, 5-15 parts of pyrolysis resin, 0.5-2 parts of plasticizer and 0.1-3 parts of dispersant; the preparation method of the binder comprises the steps of (1) weighing the components, (2) stirring at high temperature, and (3) crushing and granulating; the binder is used for preparing alumina or zirconia thermal degreasing injection molding ceramics, an injection ceramic blank body using the binder can be directly subjected to thermal degreasing in the whole process, the feeding surface is smooth, the green blank strength is high, the fluidity is good, the automatic production is easy, and the prepared injection molding ceramic product has the advantages of few pores, high density, high hardness and strength and excellent comprehensive performance.
Description
Technical Field
The invention belongs to the field of ceramic materials, and particularly relates to a binder and a preparation method and application thereof.
Background
The ceramic injection molding technology is a relatively new near-net-shape molding technology developed in recent ten years, is increasingly applied in the ceramic industry, has the characteristics of one-time molding of products with complex shapes, high product size precision, no need of mechanical processing or only need of micro processing, easiness in realization of production automation, excellent product performance and the like, is suitable for manufacturing ceramic parts in large batch, and makes up for the defects of the traditional ceramic molding process.
However, since the ceramic powder particles are basically nano or submicron powder, especially zirconia and alumina ceramics, and have the characteristics of small powder particle size, high specific surface area, irregular shape, hydrophilic surface and the like, the ceramic powder particles are difficult to disperse and mix in the thermoplastic binder, and the ceramic feed with low viscosity, high dispersion and high loading capacity is difficult to prepare. Meanwhile, as the ceramic powder particles are small and the particle stacking pores are small, the blank body is difficult to form a communicated glue discharging pore channel, the glue discharging time of ceramic injection molding is long, the ceramic injection molding is easy to foam, crack and deform, and the like, and the problem of glue discharging is solved, so that the key of ceramic injection molding is solved.
At present, the relatively mature ceramic injection molding adhesive mainly adopts a thermoplastic adhesive, and the important components of the thermoplastic adhesive are based on low molecular components, wax or various oil substances, including various low molecular and low melting point components such as paraffin, microcrystalline wax, palm wax, beeswax, peanut oil, edible oil and the like; the skeleton component is polyethylene, polypropylene, ethylene-vinyl acetate copolymer and polystyrene; and a dispersing agent, a coupling agent, a plasticizer, a release agent and the like are added. The thermoplastic binder is added with a large amount of low molecular organic components, such as wax, stearic acid, vegetable oil, oleic acid, plasticizer and the like, so that the low molecular organic components have extremely low melting points and are easily dissolved in organic solvents, the proportion of the low molecular organic components in the binder is more than 50 percent, and some formulations even reach more than 70 percent, so that the binder is easy to obtain low-viscosity and high-fluidity feed, but the thermoplastic binder has the following defects in the long-term use process: (1) the low molecular components are too many, and injection defects such as shrinkage cavity, surface bubbling, welding marks and the like are easy to generate; (2) the prepared green body has low strength, the tailing is difficult to separate, and the automatic production is difficult to realize; (3) in the solvent degreasing process, the macromolecular swelling phenomenon is easy to generate, and particles are easy to rearrange, so that the binder removal bubbling, cracking and size deformation are caused; (4) a large amount of organic solvent is needed in the rubber discharging process, so that the environment is not protected; (5) because the low-melting-point component of the binder has high occupation ratio, particle rearrangement can be generated in the processes of solvent degreasing and thermal degreasing, micro pores are more due to local agglomeration, and the strength of a sintered blank is low.
Disclosure of Invention
One of the purposes of the invention is to provide a binder, which comprises the following components in parts by weight: 3-10 parts of low molecular weight wax component, 20-50 parts of 1# polyacrylic resin, 0-30 parts of 2# polyacrylic resin, 5-35 parts of pyrolysis resin, 0.5-2 parts of plasticizer and 0.1-3 parts of dispersant.
Preferably, the content of the low molecular weight wax component is 3-5 parts, and the low molecular weight wax component is one or two or more of paraffin, microcrystalline wax and beeswax.
The low molecular weight wax has low viscosity, good fluidity and decomposition temperature mainly between 180 ℃ and 220 ℃, and the low molecular weight wax components are firstly thermally decomposed except the plasticizer and the dispersant with low content, and the content of the wax components is not more than 10 percent, thereby avoiding the risk of cracking a blank body caused by the decomposition of a large amount of wax in a narrow temperature range when the direct thermal degreasing is carried out due to the high content of the wax.
Preferably, the polyacrylic resin No. 1 has a molecular weight of 120000-400000 and a glass transition temperature Tg of 60-110 ℃, the polyacrylic resin No. 1 has a thermal decomposition temperature of 200-260 ℃, and the polyacrylic resin No. 1 can be controlled by Tg design (by polymerization or monomer, the Tg glass transition temperature of the synthetic resin is controlled) and molecular weight control.
The No. 1 polyacrylic resin is purchased by import, belongs to macromolecule cracking, has good decomposition performance, can be decomposed gradually, is different from paraffin which forms liquid phase at the melting point and above, and avoids the problems of powder particle rearrangement, powder local agglomeration, glue discharging deformation, cracking, air hole generation and strength reduction during sintering, which are caused by the capillary action.
Preferably, the 2# polyacrylic resin is a polyacrylic resin with the molecular weight of 10000-100000 and the glass transition temperature Tg of 0-60 ℃, and the thermal decomposition temperature of the 2# polyacrylic resin is 250-300 ℃.
The No. 2 polyacrylic resin is purchased for import, has a wider thermal decomposition temperature range, is gradually thermally decomposed to remove the binder, and can be effectively communicated with a glue discharging pore channel.
Preferably, the pyrolysis resin is one, two or more of polypropylene (PP), Polyethylene (PE), ethylene-vinyl acetate copolymer (EVA) and Polystyrene (PS).
The decomposition temperature of the PP is 300-350 ℃, the decomposition temperature of the PE is 380-450 ℃, the rapid decomposition temperatures of the EVA are 300-350 ℃ and 400-450 ℃, respectively, and the decomposition temperature of the PS is 250-350 ℃.
Preferably, the plasticizer is one or both of dioctyl phthalate (DOP) and dibutyl phthalate (DBP).
Preferably, the dispersant is an anionic polyacrylic dispersant.
The polyacrylic acid No. 1 and the polyacrylic acid No. 2 have good fluidity, have a large number of carboxyl groups, and can generate good compatibility with hydrophilic ceramic powder through a specially designed functional group, so that a feed with uniform mixing, high loading capacity and low viscosity is obtained, and meanwhile, at a key initial glue discharging stage of 200-300 ℃, the polyacrylic acid No. 1 and the polyacrylic acid No. 2 have good successive decomposition characteristics, can quickly and effectively form a communicated glue discharging pore channel, and are favorable for the separation of a binder.
The invention also provides a preparation method of the adhesive, which comprises the following steps:
(1) weighing the following components: weighing the components of the binder according to the weight ratio;
(2) stirring at high temperature: putting the components of the binder in the step (1) into a double-helix high-temperature mixer, stirring and mixing for 0.5-4h at the temperature of 120-180 ℃, wherein the stirring speed is 600-1000 r/min, pouring the mixture into a cooling disc after uniformly stirring at high temperature, and naturally cooling and crystallizing;
(3) crushing and granulating: and (3) pouring the cooled and crystallized binder in the step (2) into a ceramic crusher, crushing the binder into particles with the diameter of 0.5mm-5mm, and packaging and storing the particles.
It is a further object of the present invention to provide the use of the above binder in the injection molding of thermally degreased ceramics, preferably for the preparation of alumina or zirconia injection molded ceramics.
The preparation method of the alumina or zirconia injection molding ceramic comprises the following steps:
(1) placing the injection molding feed into an internal mixer, setting the temperature to be 140-190 ℃, kneading for 0.5-4h, reducing the temperature by 10-50 ℃, and continuing kneading for 0.5-2 h to obtain a mixture;
the injection molding feed comprises an alumina feed or a zirconia feed, wherein the alumina feed comprises 80.5-90 parts by weight of alumina powder and 10-19.5 parts by weight of binder, and the zirconia feed comprises 80.5-90 parts by weight of zirconia powder and 10-19.5 parts by weight of binder.
(2) Adding the mixture subjected to banburying in the step (1) into a screw extrusion granulator, setting the temperature to be 90-160 ℃, the rotating speed of a screw to be 100-600 rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to obtain an injection green body;
(3) putting the injection blank prepared in the step (2) into a thermal degreasing and glue discharging furnace, and performing multi-stage variable-temperature glue discharging by utilizing the difference of thermal decomposition temperature zones of all components of the adhesive;
the variable-temperature glue discharging parameters are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging;
(4) placing the injection blank subjected to the glue discharging in the step (3) into a high-temperature sintering furnace, and sintering at high temperature for 1-5 hours to obtain an injection ceramic finished product;
the injection blank comprises an alumina injection blank or a zirconia injection blank, the sintering temperature of the alumina injection blank is 1528-1620 ℃, and the sintering temperature of the zirconia injection blank is 1400-1450 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the proportion of low molecular weight wax components is obviously reduced, and the modified polyacrylic resin with excellent thermal decomposition performance is adopted, so that different decomposition and cracking temperatures can be flexibly designed according to different molecular weights and types;
(2) the whole process can be directly subjected to thermal degreasing, and a glue discharging pore channel is not required to be degreased by a solvent;
(3) the high-molecular polymer with large proportion is adopted, the feeding surface is smooth, the green strength is high, the fluidity is good, and the automatic production is easy to realize;
(4) the binder removal process of stepwise thermal decomposition of each component is adopted, each component is gradually and slowly decomposed, rearrangement and agglomeration of ceramic particles are avoided, and the prepared ceramic product has few pores and high strength.
Drawings
FIG. 1 is a DSC-TG curve of # 1 acrylic resin, wherein the thermal decomposition temperature ranges are as shown in the figure: 200-260 ℃;
FIG. 2 is a DSC-TG curve of # 2 acrylic resin, wherein the thermal decomposition temperature ranges are as shown in the figure: 250 to 300 ℃.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. The following examples are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of the invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
Weighing the following components in parts by weight: 7 parts of microcrystalline wax, 40 parts of No. 1 polyacrylic resin, 30 parts of No. 2 polyacrylic resin, 20 parts of PS, 1.5 parts of DOP and 1.5 parts of dispersing agent.
The No. 1 polyacrylic resin is a polyacrylic resin with the molecular weight of 120000 and the Tg of 110 ℃, and the thermal decomposition temperature is 235 ℃; the No. 2 polyacrylic resin is polyacrylic resin with the molecular weight of 40000 and the Tg of 35 ℃, the thermal decomposition temperature is 280 ℃, the decomposition temperature of PS is 320 ℃, and the dispersing agent is an anionic polyacrylic dispersing agent.
Putting the weighed materials into a double-helix high-temperature mixer, stirring and mixing for 4 hours at the temperature of 120 ℃, wherein the stirring speed is 1000 r/min, pouring the materials into a cooling disc after uniformly stirring at high temperature, naturally cooling and crystallizing, pouring the cooled and crystallized binder into a ceramic crusher, crushing the binder into particles with the diameter of 1mm, and packaging and storing the particles.
Example 2
Weighing the following components in parts by weight: 10 parts of microcrystalline wax, 45 parts of No. 1 polyacrylic resin, 35 parts of PS, 5 parts of EVA, 1.5 parts of DOP and 3.5 parts of dispersing agent.
The No. 1 polyacrylic resin is the polyacrylic resin with the molecular weight of 200000 and the Tg of 65 ℃, and the thermal decomposition temperature is 245 ℃; the decomposition temperature of the PS is 325 ℃, and the decomposition temperature of the EVA is 420 ℃. The dispersant is anionic polyacrylic acid dispersant.
Putting the weighed materials into a double-helix high-temperature mixer, stirring and mixing for 3 hours at the temperature of 140 ℃, wherein the stirring speed is 900 revolutions per minute, pouring the materials into a cooling disc after uniformly stirring at high temperature, naturally cooling and crystallizing, pouring the cooled and crystallized binder into a ceramic crusher, crushing the binder into particles with the diameter of 2mm, and packaging and storing the particles.
Example 3
Weighing the following components in parts by weight: 5 parts of microcrystalline wax, 47 parts of No. 1 polyacrylic resin, 35 parts of PS, 7 parts of EVA, 2.5 parts of DOP and 3.5 parts of dispersing agent.
The No. 1 polyacrylic resin is polyacrylic resin with the molecular weight of 400000 and the Tg of 105 ℃, and the thermal decomposition temperature is 210 ℃; the decomposition temperature of the PS is 325 ℃, and the decomposition temperature of the EVA is 420 ℃. The dispersant is anionic polyacrylic acid dispersant.
Putting the weighed materials into a double-helix high-temperature mixer, stirring and mixing for 2 hours at the temperature of 160 ℃, wherein the stirring speed is 800 revolutions per minute, pouring the materials into a cooling disc after uniformly stirring at high temperature, naturally cooling and crystallizing, pouring the cooled and crystallized binder into a ceramic crusher, crushing the binder into particles with the diameter of 3mm, and packaging and storing the particles.
Example 4
Weighing the following components in parts by weight: 5 parts of microcrystalline wax, 35 parts of No. 1 polyacrylic resin, 25 parts of No. 2 polyacrylic resin, 15 parts of PS, 15 parts of EVA, 1.5 parts of DOP and 3.5 parts of dispersing agent.
The No. 1 polyacrylic resin is the polyacrylic resin with the molecular weight of 160000 and the Tg of 80 ℃, and the thermal decomposition temperature is 230 ℃; the No. 2 polyacrylic resin is a polyacrylic resin with the molecular weight of 26000 and the Tg of 26 ℃, the thermal decomposition temperature is 285 ℃, the decomposition temperature of PS is 325 ℃, and the decomposition temperature of EVA is 420 ℃. The dispersant is anionic polyacrylic acid dispersant.
Putting the weighed materials into a double-helix high-temperature mixer, stirring and mixing for 1h at the temperature of 180 ℃, wherein the stirring speed is 700 r/min, pouring the materials into a cooling disc after uniformly stirring at high temperature, naturally cooling and crystallizing, pouring the cooled and crystallized binder into a ceramic crusher, crushing the binder into particles with the diameter of 4mm, and packaging and storing the particles.
Application example 1
Weighing the following components in parts by weight: the particle size is 1 μm, the specific surface area is 20 m281 parts per g of high-purity aluminum oxide powder and 19 parts of the binder prepared in example 1.
Placing the prepared component materials into an internal mixer, setting the temperature to be 160 ℃, kneading for 3 hours, reducing the temperature by 30 ℃, and continuing to knead for 1 hour; adding the material after the milling kneading into a screw extrusion granulator, setting the temperature at 160 ℃, the rotating speed of the screw at 400rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to prepare an injection blank; directly putting the injection blank into a hot degreasing and glue discharging furnace for discharging glue, wherein the parameters of the glue discharging furnace are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging; and (3) placing the injection blank subjected to high-temperature binder removal into a high-temperature sintering furnace, and sintering at 1600 ℃ for 3h to obtain the alumina ceramic.
Application example 2
Weighing the following components in parts by weight: the particle size is 1 μm, the specific surface area is 2m283 parts per g of highly pure aluminum oxide powder, Binder prepared in example 2And 17 parts.
Placing the prepared component materials into an internal mixer, setting the temperature to be 150 ℃, kneading for 3 hours, reducing the temperature by 30 ℃, and continuing to knead for 1 hour; adding the material after the milling kneading into a screw extrusion granulator, setting the temperature at 150 ℃, the rotating speed of the screw at 400rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to prepare an injection blank; directly putting the injection blank into a hot degreasing and glue discharging furnace for discharging glue, wherein the parameters of the glue discharging furnace are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging; and (3) placing the injection blank subjected to high-temperature binder removal into a high-temperature sintering furnace, and sintering at 1600 ℃ for 3h to obtain the alumina ceramic.
Application example 3
Weighing the following components in parts by weight: the particle size is 0.5 μm, the specific surface area is 15 m285 parts of high-purity zirconia powder per gram and 15 parts of the binder prepared in example 3.
Placing the prepared component materials into an internal mixer, setting the temperature to be 155 ℃, kneading for 3 hours, reducing the temperature by 30 ℃, and continuing to knead for 1 hour; adding the material after the milling kneading into a screw extrusion granulator, setting the temperature at 155 ℃, the rotating speed of the screw at 400rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to prepare an injection blank; directly putting the injection blank into a hot degreasing and glue discharging furnace for discharging glue, wherein the parameters of the glue discharging furnace are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging; and (3) placing the injection blank subjected to high-temperature binder removal into a high-temperature sintering furnace, and sintering at 1420 ℃ for 3h to obtain the zirconia ceramic.
Application example 4
Weighing the following components in parts by weight: the particle size is 0.2 μm, the specific surface area is 7 m284 parts of high-purity zirconia powder per gram and 16 parts of the binder prepared in example 4.
Placing the prepared component materials into an internal mixer, setting the temperature to be 160 ℃, kneading for 3 hours, reducing the temperature by 30 ℃, and continuing to knead for 1 hour; adding the material after the milling kneading into a screw extrusion granulator, setting the temperature at 160 ℃, the rotating speed of the screw at 400rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to prepare an injection blank; directly putting the injection blank into a hot degreasing and glue discharging furnace for discharging glue, wherein the parameters of the glue discharging furnace are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging; and (3) placing the injection blank subjected to high-temperature binder removal into a high-temperature sintering furnace, and sintering at 1420 ℃ for 3h to obtain the zirconia ceramic.
According to the hardness test standard: the test method GB/T16534-: the main detection data of the detection basis in the fine ceramic room temperature hardness test method GB/T6568-2006 are shown in the following table 1:
table 1 shows the performance indexes of the injection ceramics prepared in application examples 1 to 4
Selecting a binder | Density/g/cm3 | hardness/HV | Three-point bending strength/Mpa | Appearance after polishing | |
Application example 1 | Example 1 | 3.925 | 1680 | 443.5 | Pore-free |
Application example 2 | Example 2 | 3.928 | 1690 | 446.7 | Pore-free |
Application example 3 | Example 3 | 6.075 | 1250 | 785 | Pore-free |
Application example 4 | Example 4 | 6.077 | 1255 | 788 | Pore-free |
As can be seen from Table 1, by applying the binder of examples 1 to 4, the prepared alumina injection ceramic and zirconia injection ceramic both have high density, hardness and strength, and the polished surfaces have no pores and excellent performance indexes.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. 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 (4)
1. The adhesive is characterized by comprising the following components in parts by weight: 3-7 parts of low molecular weight wax component, 45-50 parts of No. 1 polyacrylic resin, 25-30 parts of No. 2 polyacrylic resin, 5-15 parts of pyrolysis resin, 0.5-2 parts of plasticizer and 0.1-3 parts of dispersant;
the low molecular weight wax component is one or two or more of paraffin, microcrystalline wax and beeswax;
the No. 1 polyacrylic resin is a polyacrylic resin with the molecular weight of 200000-400000 and the glass transition temperature Tg of 60-110 ℃, and the thermal decomposition temperature of the No. 1 polyacrylic resin is 200-260 ℃;
the 2# polyacrylic resin is a polyacrylic resin with the molecular weight of 10000-100000 and the glass transition temperature Tg of 0-60 ℃, and the thermal decomposition temperature of the 2# polyacrylic resin is 250-300 ℃;
the high-temperature decomposition resin is one or two of polypropylene (PP) and Polyethylene (PE);
the plasticizer is one or two of dioctyl phthalate (DOP) or dibutyl phthalate (DBP);
the dispersant is anionic polyacrylic acid dispersant.
2. A method of preparing the binder of claim 1, wherein the method comprises the steps of:
(1) weighing the following components: weighing the components of the binder according to the weight ratio;
(2) stirring at high temperature: putting the components of the binder in the step (1) into a double-helix high-temperature mixer, stirring and mixing for 0.5-4h at the temperature of 120-180 ℃, wherein the stirring speed is 600-1000 r/min, pouring the mixture into a cooling disc after uniformly stirring at high temperature, and naturally cooling and crystallizing;
(3) crushing and granulating: and (3) pouring the cooled and crystallized binder in the step (2) into a ceramic crusher, crushing the binder into particles with the diameter of 0.5mm-5mm, and packaging and storing the particles.
3. Use of a binder according to claim 1 for the preparation of an alumina or zirconia injection molded ceramic for the injection molding of a thermally degreased ceramic.
4. The method of making an injection molded ceramic according to claim 3, comprising the steps of:
(1) putting the injection molding feed into an internal mixer, setting the temperature to be 140-190 ℃, kneading for 0.5-4h, reducing the temperature by 10-50 ℃, and continuing kneading for 0.5-2 h to obtain a mixture;
the injection molding feed is an alumina feed or a zirconia feed, the alumina feed consists of 80.5-90 parts by weight of alumina powder and 10-19.5 parts by weight of binder, and the zirconia feed consists of 80.5-90 parts by weight of zirconia powder and 10-19.5 parts by weight of binder; the binder is the binder of claim 1;
(2) adding the mixture subjected to banburying in the step (1) into a screw extrusion granulator, setting the temperature to be 90-160 ℃, the rotating speed of a screw to be 100-600 rpm, granulating to obtain hot degreased ceramic injection molding feed particles, putting the feed particles on a ceramic injection molding machine, and performing injection molding to obtain an injection green body;
(3) putting the injection blank prepared in the step (2) into a thermal degreasing and glue discharging furnace, and performing multi-stage variable-temperature glue discharging by utilizing the difference of thermal decomposition temperature zones of all components of the adhesive;
the variable-temperature glue discharging parameters are as follows: heating the temperature from room temperature to 150 ℃ at the speed of 2 ℃/min, heating the temperature to 200 ℃ at the speed of 1 ℃/min, heating the temperature to 250 ℃ at the speed of 0.2 ℃/min, preserving the heat for 3h, heating the temperature to 300 ℃ at the speed of 0.3 ℃/min, preserving the heat for 2h, heating the temperature to 400 ℃ at the speed of 0.5 ℃/min, preserving the heat for 2h, heating the temperature to 500 ℃ at the speed of 1 ℃/min, preserving the heat for 2h, heating the temperature to 800 ℃ at the speed of 1.5 ℃/min, preserving the heat for 2h, stopping heating, and naturally cooling the temperature to room temperature to finish high-temperature glue discharging;
(4) placing the injection blank subjected to the glue discharging in the step (3) into a high-temperature sintering furnace, and sintering at high temperature for 1-5 hours to obtain an injection ceramic finished product;
the injection green body is an alumina injection green body or a zirconia injection green body, the sintering temperature of the alumina injection green body is 1528-1620 ℃, and the sintering temperature of the zirconia injection green body is 1400-1450 ℃.
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JPH01153569A (en) * | 1987-12-08 | 1989-06-15 | Nippon Denso Co Ltd | Binder for injection molding of ceramic |
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JPH01153569A (en) * | 1987-12-08 | 1989-06-15 | Nippon Denso Co Ltd | Binder for injection molding of ceramic |
CN1291538A (en) * | 1999-09-10 | 2001-04-18 | 精工电子有限公司 | Shaping method of ceramics |
CN105236963A (en) * | 2015-09-10 | 2016-01-13 | 卢立建 | Zirconium oxide ceramic ferrule workblank production process |
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