CN103833373A - Environment-friendly production method for nanometer ultrafine ceramic - Google Patents
Environment-friendly production method for nanometer ultrafine ceramic Download PDFInfo
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- CN103833373A CN103833373A CN201410000668.6A CN201410000668A CN103833373A CN 103833373 A CN103833373 A CN 103833373A CN 201410000668 A CN201410000668 A CN 201410000668A CN 103833373 A CN103833373 A CN 103833373A
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Abstract
The invention relates to the field of ceramic preparation, especially to an environment-friendly production method for a nanometer ultrafine ceramic. The production method comprises the following steps: (1) subjecting polyvinyl butyral and polyethylene glycol to mixing so as to obtain a uniform mixture, thereby obtaining a water-based forming agent; (2) mixing the water-based forming agent with ceramic powder, heating the obtained mixture and subjecting the heated mixture to internal mixing in an internal mixer so as to obtain uniform pug; (3) subjecting the pug obtained after internal mixing to fragmentation or extrusion granulation so as to obtain a feed with uniform particles; (4) injecting the feed into an injection machine and carrying out injection molding in an injection mold so as to obtain a ceramic injection green body; (5) putting the ceramic injection green body into water, carrying out heating and heat preservation and removing polyethylene glycol; (6) sintering the ceramic injection green body having undergone water extraction; and (7) cooling an extracted aqueous polyethylene glycol solution and carrying out centrifugal dewatering. According to the invention, the water-based forming agent is used to replace paraffin used in conventional production process, polyethylene glycol is removed by using hot water before sintering, so resources are saved, and the environment is greatly improved.
Description
Technical field
The present invention relates to ceramics processing field, particularly the environment-protection production method of the ultra-fine pottery of a kind of nanometer.
Background technology
Ceramic is widely used in industry, the technical field such as civilian, well known common, as LED lamp holder, for motor car engine, the component of sparking plug, microwave oven electric heater are produced, and all use pottery.The production method of existing pottery is hot pressing note, and paraffin becomes mobile slurry with ceramic powder consolute, moulding on Hot-pressed injector, then burning dewaxing, then high temperature sintering.Existing ceramics injection note technique, because of the dewaxing of will burning, the burning of a large amount of paraffin heat, causes a large amount of paraffin wastes, more seriously, and great amount of carbon dioxide discharge, air, water are seriously polluted.According to statistics, 1 year up to ten million ton of national paraffin hot-injection molding ceramic, within 1 year, discharge carbonic acid gas is more than 1,000,000 tons.Traditional pottery manufacture is polluted and has been reached very serious stage the impact of the area surroundings such as Foshan, production base, Yixing, Henan, Hebei, newization of Hunan.Therefore the environment-protection production method of developing a kind of pottery has become the focus of industry research.
Summary of the invention
For the deficiency of above-mentioned prior art existence, the object of this invention is to provide the environment-protection production method of the ultra-fine pottery of a kind of nanometer, it is simple that it has technique, workable, the feature of energy-conserving and environment-protective.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The environment-protection production method of the ultra-fine pottery of a kind of nanometer of the present invention, comprises the steps:
(1) the preparation of base molded dose: by mixing the polyoxyethylene glycol of the polyvinyl butyral acetal of 10-30 mass parts and 70-90 mass parts become uniform mixture, obtain water base forming agent;
(2) batch mixing: by step (1) in the water base forming agent of gained mix with ceramic powder, intensification, in Banbury mixer, banburying becomes uniform pug;
(3) granulation: the feeding that the pug fragmentation of banburying or extruding pelletization is become to single-size;
(4) injection molding: feeding injection is added in injection moulding machine, and injection moulding in the injection mold of injection moulding machine, obtains ceramic member injection base;
(5) degreasing: ceramic member is injected to base and put into water, by water heating and thermal insulation, the polyoxyethylene glycol that ceramic member is injected in base removes;
(6) sintering: the ceramic member injection base after water extraction is pressed to traditional method sintering in ceramic sintering furnace;
(7) recycling of Aqueous Solutions of Polyethylene Glycol: by the Aqueous Solutions of Polyethylene Glycol cooling of extraction, in supercentrifuge, water is removed, polyoxyethylene glycol is separated from water.
Wherein, step (1) described in melting temperature be 150 DEG C.
Wherein, step (2) described in ceramic powder be Al
2o
3,zrO
2, TiC, SiO
2or TiB
2in one or more composite powders, the particle diameter of described ceramic powder is 0.1um-5um.
Wherein, step (2) described in water base forming agent and ceramic powder in mass ratio the ratio of 15-25:75-85 mix, described intensification temperature is 180 DEG C.
Wherein, step (3) described in the particle diameter of feeding be 2-3mm.
Wherein, step (4) described in injection temperature be 150 DEG C-180 DEG C, described injection pressure is 60-100KPa.
Wherein, step (5) described in water heating and thermal insulation temperature be 50-70 DEG C, soaking time 8-12 hour.
Wherein, step (6) described in sintering temperature be 1500-1800 DEG C; In described sintering temperature, lower than 800 DEG C, heat-up rate is 4 DEG C/min, and in described sintering temperature, higher than 800 DEG C, heat-up rate is 5 DEG C/min.
Wherein, step (7) described in Aqueous Solutions of Polyethylene Glycol cool to 10 DEG C.
Wherein, step (1) described in the molecular weight of polyvinyl butyral acetal be 4-10 ten thousand, the molecular weight of described polyoxyethylene glycol is 2000-4000.
Compared with prior art, there is following features in the present invention:
1, base molded dose of paraffin substituting in existing production technique of water of the present invention, and before sintering, adopt hot water that polyoxyethylene glycol is removed, and recyclable re-using, not only effectively saved resource, what is more important has greatly been improved environmental factors, has reduced air, water pollution.
2, the present invention adopts advanced injection molding technology to replace traditional hot pressing injecting method, and workman's production environment is improved, and labour intensity reduces.
3, base molded dose of injection blank of water of the present invention is more even than cerul pressure injection base density, and after degreasing, subsurface defect greatly reduces.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
Getting molecular weight is that the polyvinyl butyral acetal 2.5Kg of 4-10 ten thousand and the polyoxyethylene glycol 7.5Kg of molecular weight 2000-4000 mix, and is warming up to after 150 DEG C, and the uniform mixture of mixing one-tenth, obtains water base forming agent; In above-mentioned water base forming agent, add Al
2o
3powder 40Kg(Al
2o
3the particle diameter 0.1um-5um of powder) mix, be warmed up to 180 DEG C, in Banbury mixer, banburying becomes uniform pug; The pug fragmentation of banburying or extruding pelletization are become to the feeding (particle diameter 2-3mm) of single-size; Feeding injection is added in injection moulding machine (each section of temperature of injection moulding machine is controlled between 150 DEG C-180 DEG C), and injection moulding in the injection mold (injection pressure is controlled at 60-100KPa) of injection moulding machine, obtains ceramic member injection base; Ceramic member is injected to base and put into water, heat water to 50 DEG C, be incubated 12 hours, the most of polyoxyethylene glycol in ceramic member injection base will be dissolved in water; By the ceramic member injection base after water extraction in ceramic sintering furnace sintering (sintering temperature is 1500-1800 DEG C; In described sintering temperature, lower than 800 DEG C, heat-up rate is 4 DEG C/min, the binder removal that heats up at a slow speed at low temperatures, and in described sintering temperature, higher than 800 DEG C, heat-up rate is 5 DEG C/min, sintering is at high temperature rapidly heated); Aqueous Solutions of Polyethylene Glycol after extraction is cooled to 10 DEG C, in supercentrifuge, water is removed, polyoxyethylene glycol is separated from water, water and polyoxyethylene glycol all be can be recycled.
Embodiment 2
Getting molecular weight is that the polyvinyl butyral acetal 1Kg of 4-10 ten thousand and the polyoxyethylene glycol 9Kg of molecular weight 2000-4000 mix, and is warming up to after 150 DEG C, and the uniform mixture of mixing one-tenth, obtains water base forming agent; In above-mentioned water base forming agent, add TiC and ZrO
2the particle diameter 0.1um-5um of powder 50Kg(mixed powder) mix, be warmed up to 180 DEG C, in Banbury mixer, banburying becomes uniform pug; The pug fragmentation of banburying or extruding pelletization are become to the feeding (particle diameter 2-3mm) of single-size; Feeding injection is added in injection moulding machine (each section of temperature of injection moulding machine is controlled between 150 DEG C-180 DEG C), and injection moulding in the injection mold (injection pressure is controlled at 60-100KPa) of injection moulding machine, obtains ceramic member injection base; Ceramic member is injected to base and put into water, heat water to 60 DEG C, be incubated 10 hours, the most of polyoxyethylene glycol in ceramic member injection base will be dissolved in water; By the ceramic member injection base after water extraction in ceramic sintering furnace sintering (described sintering temperature is 1500-1800 DEG C; In described sintering temperature, lower than 800 DEG C, heat-up rate is 4 DEG C/min, the binder removal that heats up at a slow speed at low temperatures, and in described sintering temperature, higher than 800 DEG C, heat-up rate is 5 DEG C/min, sintering is at high temperature rapidly heated); Aqueous Solutions of Polyethylene Glycol after extraction is cooled to 10 DEG C, in supercentrifuge, water is removed, polyoxyethylene glycol is separated from water, water and polyoxyethylene glycol all be can be recycled.
Embodiment 3
Getting molecular weight is that the polyvinyl butyral acetal 3Kg of 4-10 ten thousand and the polyoxyethylene glycol 7Kg of molecular weight 2000-4000 mix, and is warming up to after 150 DEG C, and the uniform mixture of mixing one-tenth, obtains water base forming agent; In above-mentioned water base forming agent, add SiO
2and TiB
2the particle diameter 0.1um-5um of powder 40Kg(mixed powder) mix, be warmed up to 180 DEG C, in Banbury mixer, banburying becomes uniform pug.The pug fragmentation of banburying or extruding pelletization are become to the feeding (particle diameter 2-3mm) of single-size.Feeding injection is added in injection moulding machine (each section of temperature of injection moulding machine is controlled between 150 DEG C-180 DEG C), and injection moulding in the injection mold (injection pressure is controlled at 60-100KPa) of injection moulding machine, obtains ceramic member injection base; Ceramic member is injected to base and put into water, heat water to 70 DEG C, be incubated 8 hours, the most of polyoxyethylene glycol in ceramic member injection base will be dissolved in water; Ceramic member injection base after water extraction is pressed to traditional method sintering in ceramic sintering furnace.By the ceramic member injection base after water extraction in ceramic sintering furnace sintering (described sintering temperature is 1500-1800 DEG C; In described sintering temperature, lower than 800 DEG C, heat-up rate is 4 DEG C/min, the binder removal that heats up at a slow speed at low temperatures, and in described sintering temperature, higher than 800 DEG C, heat-up rate is 5 DEG C/min, sintering is at high temperature rapidly heated); Aqueous Solutions of Polyethylene Glycol after extraction is cooled to 10 DEG C, in supercentrifuge, water is removed, polyoxyethylene glycol is separated from water, water and polyoxyethylene glycol all be can be recycled.
The above is only preferred embodiments of the present invention, and the equivalence of making according to the technological principle described in patent claim of the present invention therefore all changes or amendment, is included in patent claim of the present invention.
Claims (10)
1. an environment-protection production method for the ultra-fine pottery of nanometer, is characterized in that, comprises the steps:
(1) the preparation of water base forming agent: by mixing the polyoxyethylene glycol of the polyvinyl butyral acetal of 10-30 mass parts and 70-90 mass parts become uniform mixture, obtain water base forming agent;
(2) batch mixing: by step (1) in the water base forming agent of gained mix with ceramic powder, intensification, in Banbury mixer, banburying becomes uniform pug;
(3) granulation: the feeding that the pug fragmentation of banburying or extruding pelletization is become to single-size;
(4) injection molding: feeding injection is added in injection moulding machine, and injection moulding in the injection mold of injection moulding machine, obtains ceramic member injection base;
(5) degreasing: ceramic member is injected to base and put into water, by water heating and thermal insulation, the polyoxyethylene glycol that ceramic member is injected in base removes;
(6) sintering: by the ceramic member injection base sintering in ceramic sintering furnace after water extraction;
(7) recycling of Aqueous Solutions of Polyethylene Glycol: by the Aqueous Solutions of Polyethylene Glycol cooling of extraction, in supercentrifuge, water is removed, polyoxyethylene glycol is separated from water.
2. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (1) described in melting temperature be 150 DEG C.
3. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (2) described in ceramic powder be Al
2o
3,zrO
2, TiC, SiO
2or TiB
2in one or more composite powders, the particle diameter of described ceramic powder is 0.1um-5um.
4. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (2) described in water base forming agent and ceramic powder in mass ratio the ratio of 15-25:75-85 mix, described intensification temperature is 180 DEG C.
5. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (3) described in the particle diameter of feeding be 2-3mm.
6. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (4) described in injection temperature be 150 DEG C-180 DEG C, described injection pressure is 60-100KPa.
7. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (5) described in water heating and thermal insulation temperature be 50-70 DEG C, soaking time 8-12 hour.
8. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (6) described in sintering temperature be 1500-1800 DEG C; In described sintering temperature, lower than 800 DEG C, heat-up rate is 4 DEG C/min, and in described sintering temperature, higher than 800 DEG C, heat-up rate is 5 DEG C/min.
9. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (7) described in Aqueous Solutions of Polyethylene Glycol cool to 10 DEG C.
10. the environment-protection production method of the ultra-fine pottery of nanometer according to claim 1, is characterized in that: step (1) described in the molecular weight of polyvinyl butyral acetal be 4-10 ten thousand, the molecular weight of described polyoxyethylene glycol is 2000-4000.
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|---|---|---|---|
| CN201410000668.6A CN103833373A (en) | 2014-01-02 | 2014-01-02 | Environment-friendly production method for nanometer ultrafine ceramic |
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|---|---|---|---|
| CN201410000668.6A CN103833373A (en) | 2014-01-02 | 2014-01-02 | Environment-friendly production method for nanometer ultrafine ceramic |
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| CN103833373A true CN103833373A (en) | 2014-06-04 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017120990A1 (en) * | 2016-01-13 | 2017-07-20 | 广东工业大学 | Process for preparing net-size, complex-shape transparent ceramic piece |
| CN110742314A (en) * | 2019-10-22 | 2020-02-04 | 深圳羽制科技有限公司 | Electronic cigarette atomization core porous ceramic and preparation method thereof |
| CN113105216A (en) * | 2021-04-07 | 2021-07-13 | 盐城工学院 | Injection-molded zirconium-aluminum composite ceramic and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102307827A (en) * | 2009-02-09 | 2012-01-04 | 株式会社Ihi | Process for producing sintered sialon ceramic |
-
2014
- 2014-01-02 CN CN201410000668.6A patent/CN103833373A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102307827A (en) * | 2009-02-09 | 2012-01-04 | 株式会社Ihi | Process for producing sintered sialon ceramic |
Non-Patent Citations (2)
| Title |
|---|
| 刘君 等: "《无机化学实验》", 31 July 2013, 化学工业出版社 * |
| 薛大权 等: "《聚乙二醇在医药学领域的应用与技术》", 30 April 2011, 华中科技大学出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017120990A1 (en) * | 2016-01-13 | 2017-07-20 | 广东工业大学 | Process for preparing net-size, complex-shape transparent ceramic piece |
| CN110742314A (en) * | 2019-10-22 | 2020-02-04 | 深圳羽制科技有限公司 | Electronic cigarette atomization core porous ceramic and preparation method thereof |
| CN113105216A (en) * | 2021-04-07 | 2021-07-13 | 盐城工学院 | Injection-molded zirconium-aluminum composite ceramic and preparation method thereof |
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Application publication date: 20140604 |