CN103275623B - Novel high temperature resisting phosphate adhesive - Google Patents
Novel high temperature resisting phosphate adhesive Download PDFInfo
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- CN103275623B CN103275623B CN201310244976.9A CN201310244976A CN103275623B CN 103275623 B CN103275623 B CN 103275623B CN 201310244976 A CN201310244976 A CN 201310244976A CN 103275623 B CN103275623 B CN 103275623B
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Abstract
The invention discloses a novel high temperature resisting phosphate adhesive. Phosphate solution prepared through the reaction of phosphoric acid and aluminium hydroxide is adopted as a base stock, a carbon nanotube serves as a filler, AIN serves as a curing agent, and zinc oxide and magnesium oxide are added to prepare the phosphate adhesive with higher bonding strength and higher high temperature resistance. Meanwhile, the raw material for preparing is wide in sources, and is cheap and accessible, and the synthesis process is simple and easy to industrial production.
Description
Technical field
The present invention relates to a kind of sizing agent, particularly a kind of novel fire resistant Phosphate adhesive.
Background technology
People are in exploring new high-temperature material, and because phosphoric acid salt has high-melting-point, condensation polymerization, its theory and combining intensity is up to 10
4mPa, far above other combining form, so phosphoric acid salt high temperature material has been given to the attention of height.From 18 end of the centurys to 19 beginnings of the century, scientific worker's phosphate concrete that begins one's study.They,, annealed ZnO and superphosphate furnishing underflow, fill a decayed tooth and teeth space at first.Because this gelling material has solidifying, cohesive force soon, can become nontoxic hard material by force and after condensing, and result of use is good, is still odontologist's widespread use so far.Tooth is with after gelling material, and industrial high temperature kiln and other high temperature engineering also start to apply phosphate concrete, to the application forties in 20th century, increases, and gets back and further develops later.Can prepare refractory concrete or prefabricated components by methods such as tamping, vibration and half-dried compression mouldings now; Also can and the furnace lining that method is made metallurgical industry and other high temperature kiln such as smear with direct cast.The 1950's, development along with defense technology, material property has been proposed to stricter requirement, and phosphate concrete is because refractoriness is high, thermal shock resistance is good, corrosion strength is strong, electric property is superior, therefore being subject to various countries scientific worker greatly payes attention to, and carried out a large amount of experimental studies, for wide prospect has been opened up in the application of phosphate concrete in hard-core technology field.It can do heat release antioxidant coating, impact type jet engine combustion chamber solar heat protection liner, electrical apparatus insulation material, high temperature radome material, the reactor corrosion-proof paint of light heat-insulating material, rocket and supersonic plane head of high temperature resistant loss prevention coating, guided missile and the rocket high-temperature systems of launching pad cushion parts.In these application, the most important with the development of the phosphate composite material of metal or nonmetal wire, ripple bar, Honeycomb.The feature such as that phosphate composite material has is high temperature resistant, high strength, dielectric properties are excellent, anti-oxidant and good structure designability, thermal expansivity are little.It has concentrated metal and ceramic advantage, is the ideal material of high-temperature resistant low dielectric loss.
Phosphoric acid salt has the advantages such as nontoxic, tasteless, nuisanceless and good high-temperature behavior and collapsibility and comes into one's own as a kind of novel inorganic sizing agent.Compare with the agent of silicate gluing, its water tolerance is better, cure shrinkage is little, hot strength is high and can be in the curing advantage of lesser temps, can bonded metal, pottery, glass etc.Phosphate adhesive is normally comprised of base-material, filler and solidifying agent.Sometimes for some needs also will add some particular matter, as setting accelerator, acid inhibitor, whipping agent and bubble stabilizer etc.
For Phosphate adhesive, should develop environment-friendly type, functional type, tailored version sizing agent, the sizing agent using under exploitation extreme condition, produces new technology for sizing agent, bonding to 3-D technology development from two dimension, sizing agent one coating one matrix material forms complementary triangle relation.(1) improve the performance of Phosphate adhesive.In the bonding strength improving base material, improve high thermal resistance, reduce fragility, improve the emphasis that the aspects such as water tolerance are tackling key problem research.(2) high performance, multifunction, become more meticulous and intelligent, Composite future development.The sizing agent of the advantage that integrates inorganic, organic sizing agent is prepared in research.(3) because nano material has great specific surface and surface energy, can give nano composite material a series of properties, in Phosphate adhesive, adding nano material will be the emphasis that people study to improve its performance.(4) multi-functional Phosphate adhesive.When a kind of sizing agent has several functions simultaneously, the pottery that can bond again can matrix metal, timber etc., and its using value can increase greatly, so multi-functional Phosphate adhesive is glue one of the development trend of agent industry of slitting.(5) aerospace will be a new high-tech industry being on a grand scale, and spacecraft, space station and various guided missile and radar manufacture all be unable to do without sizing agent with assembling, Phosphate adhesive is with its special performance, having broad application prospects aspect military affairs, national defence, should strengthen the research of extraordinary Phosphate adhesive.
Summary of the invention
The object of the invention is the defect for existing Phosphate adhesive, a kind of more Phosphate adhesive of high bond strength, higher resistance to elevated temperatures that has is provided.
In order to realize above goal of the invention, the present invention by the following technical solutions: a kind of novel fire resistant Phosphate adhesive, comprises the component of following mass fraction: 00 part of phosphatase 11; 20～30 parts of carbon nanotubes; 30～40 parts, aluminium hydroxide; 5～10 parts of solidifying agent AIN; 10～15 parts, zinc oxide; 10～15 parts, magnesium oxide, 150～200 parts of deionized waters.
Described carbon nanotube carbon nanotube is multi-walled carbon nano-tubes, and external diameter scope is 10～20nm, and length is 20～50 μ m, adopts strong acid oxide treatment.
Since first carbon nanotube was found by Electronic Speculum expert professor Iijima of Japanese NEC from 1991, between the short more than ten years, the carbonaceous pipe of this nano-scale has just caused the broad interest of the scientific circles such as global physics, chemistry and material.Due to the special construction of carbon nanotube and excellent mechanics, electricity and optical property with and potential industrial value, make it become gradually the study hotspot of the ambits such as chemistry, physics and material, have people even it to be described as to " the black diamond of 21 century ".Carbon nanotube is the One-dimensional Quantum material with special construction (radial dimension is nanometer scale, and axial dimension can reach micron dimension), has typical stratiform hollow structure feature, and there is end cap sealing at the two ends of general pipe.The pipe shaft of carbon nanotube is director circle tubular construction, hexagonal carbon ring structure unit, consists of, and terminal cap moiety is the polygonized structure containing pentagon and hexagonal carbocyclic ring composition.The special construction of carbon nanotube, makes it as filler, join in Phosphate adhesive, can improve the resistance to elevated temperatures of Phosphate adhesive.Simultaneously adding of carbon nanotube, can improve sizing agent and the chemical bond that is sticked thing surface, thereby improve the cohesive strength of Phosphate adhesive.
Major advantage of the present invention and beneficial effect are: phosphoric acid and the aluminium hydroxide reaction of take makes phosphate solution as base-material, take carbon nanotube as filler, AIN is solidifying agent, adds zinc oxide and magnesium oxide, and prepared Phosphate adhesive has more high bond strength, higher resistance to elevated temperatures.Prepare required raw material sources extensive simultaneously, be cheaply easy to get, and synthesis technique is simple, is easy to suitability for industrialized production.
Embodiment
Below by embodiment, the present invention is further illustrated.
Embodiment mono-:
By following mass fraction, prepare raw material: 00 part of phosphatase 11; 20 parts of carbon nanotubes; 40 parts, aluminium hydroxide; 8 parts of solidifying agent AIN; 14 parts, zinc oxide; 14 parts, magnesium oxide, 150 parts of deionized waters;
By phosphoric acid and deionized water wiring solution-forming, add aluminium hydroxide, stir and be heated to 110～120 ℃, reaction 2h, obtains transparent thick base-material;
In base-material, add carbon nanotube, solidifying agent AIN, zinc oxide and magnesium oxide, stir and be heated to 130～140 ℃, reaction 5h, obtains Phosphate adhesive.
Embodiment bis-:
By following mass fraction, prepare raw material: 00 part of phosphatase 11; 26 parts of carbon nanotubes; 38 parts, aluminium hydroxide; 10 parts of solidifying agent AIN; 12 parts, zinc oxide; 12 parts, magnesium oxide, 180 parts of deionized waters;
By phosphoric acid and deionized water wiring solution-forming, add aluminium hydroxide, stir and be heated to 110～120 ℃, reaction 2h, obtains transparent thick base-material;
In base-material, add carbon nanotube, solidifying agent AIN, zinc oxide and magnesium oxide, stir and be heated to 130～140 ℃, reaction 5h, obtains Phosphate adhesive.
Embodiment tri-:
By following mass fraction, prepare raw material: 00 part of phosphatase 11; 30 parts of carbon nanotubes; 34 parts, aluminium hydroxide; 7 parts of solidifying agent AIN; 15 parts, zinc oxide; 15 parts, magnesium oxide, 200 parts of deionized waters;
By phosphoric acid and deionized water wiring solution-forming, add aluminium hydroxide, stir and be heated to 110～120 ℃, reaction 2h, obtains transparent thick base-material;
In base-material, add carbon nanotube, solidifying agent AIN, zinc oxide and magnesium oxide, stir and be heated to 130～140 ℃, reaction 5h, obtains Phosphate adhesive.
Embodiment tetra-:
By following mass fraction, prepare raw material: 00 part of phosphatase 11; 22 parts of carbon nanotubes; 30 parts, aluminium hydroxide; 5 parts of solidifying agent AIN; 10 parts, zinc oxide; 10 parts, magnesium oxide, 160 parts of deionized waters;
By phosphoric acid and deionized water wiring solution-forming, add aluminium hydroxide, stir and be heated to 110～120 ℃, reaction 2h, obtains transparent thick base-material;
In base-material, add carbon nanotube, solidifying agent AIN, zinc oxide and magnesium oxide, stir and be heated to 130～140 ℃, reaction 5h, obtains Phosphate adhesive.
Performance test:
(1) by dsc and thermogravimetry, investigate solidification value and the high thermal resistance of sizing agent;
(2) mainly by bonded ceramics test piece, survey its shearing resistance.
Test result shows: Phosphate adhesive of the present invention adds solidifying agent AIN, zinc oxide and magnesium oxide to promote to some extent the reaction of sizing agent, has reduced solidification value, can realize completely curing at 130 ℃.Thermal weight loss experiment shows that sizing agent does not have weight loss after 700 ℃ of high temperature, adds as seen carbon nanotube as filler, has increased the high-temperature stability of sizing agent, and resistance to elevated temperatures is better.The normal temperature shearing resistance of sizing agent is 5.2MPa left and right, and pyroprocessing also can reach 3.2 MPa left and right, and adding of visible carbon nanotube, has improved the cohesive strength of Phosphate adhesive.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (1)
1. a high temperature resistant Phosphate adhesive, is characterized in that comprising the component of following mass fraction: 00 part of phosphatase 11; 20～30 parts of carbon nanotubes; 30～40 parts, aluminium hydroxide; 5～10 parts of solidifying agent A1N; 10～15 parts, zinc oxide; 10～15 parts, magnesium oxide, 150～200 parts of deionized waters;
Described carbon nanotube is multi-walled carbon nano-tubes, and external diameter scope is 10～20nm, and length is 20～50 μ m, adopts strong acid oxide treatment.
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| CN201310244976.9A CN103275623B (en) | 2013-06-20 | 2013-06-20 | Novel high temperature resisting phosphate adhesive |
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| CN201310244976.9A CN103275623B (en) | 2013-06-20 | 2013-06-20 | Novel high temperature resisting phosphate adhesive |
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| CN103275623A CN103275623A (en) | 2013-09-04 |
| CN103275623B true CN103275623B (en) | 2014-10-08 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104087184B (en) * | 2014-06-12 | 2015-10-28 | 太仓市金锚化工有限公司 | A kind of high-intensity high-tenacity phosphate base sizing agent |
| CN109913135A (en) * | 2019-02-18 | 2019-06-21 | 安徽鸿智菱科技有限公司 | A kind of cable formula liquid-level floater switch high-temperature-resistant adhesive |
| CN112592664A (en) * | 2020-11-13 | 2021-04-02 | 常州晶泰新材料科技有限公司 | Graphene modified phosphate composite adhesive, preparation method thereof and application of graphene modified phosphate composite adhesive in high-temperature sensor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19804696A1 (en) * | 1998-02-06 | 1999-08-19 | Didier Werke Ag | Multicomponent adhesive for binding refractory stone |
| CN101358111A (en) * | 2008-08-27 | 2009-02-04 | 黑龙江省科学院石油化学研究院 | Phosphates adhesive and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11116899A (en) * | 1997-10-13 | 1999-04-27 | Nishimura Togyo Kk | Heat radiating inorganic adhesive |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19804696A1 (en) * | 1998-02-06 | 1999-08-19 | Didier Werke Ag | Multicomponent adhesive for binding refractory stone |
| CN101358111A (en) * | 2008-08-27 | 2009-02-04 | 黑龙江省科学院石油化学研究院 | Phosphates adhesive and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《新型铸造黏结剂——碳纳米管改性磷酸盐无机树脂的研究》;张友寿等;《第十三届全国复合材料学术会议论文集》;20041031;1044-1047 * |
| 中国科学院.《2006高技术发展报告》.《2006高技术发展报告》.科学出版社,2006,60. * |
| 张友寿等.《新型铸造黏结剂——碳纳米管改性磷酸盐无机树脂的研究》.《第十三届全国复合材料学术会议论文集》.2004,1044-1047. |
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Free format text: CORRECT: INVENTOR; FROM: LI JI TO: MA XUERONG LI JI Free format text: CORRECT: ADDRESS; FROM: 210013 NANJING, JIANGSU PROVINCE TO: 226600 NANTONG, JIANGSU PROVINCE |
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Effective date of registration: 20160706 Address after: The eleven group of Ji Qing Cun Dun tou Zhen Haian County of Jiangsu Province, Nantong City, 226600 Patentee after: Haian County Fanchang Synthetic Rubber Co. Ltd. Address before: 226600 No. 8 Yingbin Road, Haian County, Nantong, Jiangsu Patentee before: Haian Changzhou University Technology Transfer Center Co., Ltd. |