CN102775635A - Cerium hydroxide heat stabilizer and preparation method thereof - Google Patents
Cerium hydroxide heat stabilizer and preparation method thereof Download PDFInfo
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- CN102775635A CN102775635A CN2012102929704A CN201210292970A CN102775635A CN 102775635 A CN102775635 A CN 102775635A CN 2012102929704 A CN2012102929704 A CN 2012102929704A CN 201210292970 A CN201210292970 A CN 201210292970A CN 102775635 A CN102775635 A CN 102775635A
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- stabilizer
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Abstract
The invention aims to disclose a cerium hydroxide heat stabilizer and a preparation method thereof. The rare earth content of the heat stabilizer is 90-95 percent; the cerium oxide content (CeO2/TREO) of the heat stabilizer is more than or equal to 99.9 percent; the burning weightlessness amount of heat stabilizer is 5-10 percent; and the average grain diameter D50 of the heat stabilizer is 0.5-3 microns. Compared with the existing product, a silicon rubber product prepared by using the cerium hydroxide heat stabilizer has the advantages of high heat-resistant performance, good product color and the like, so that the aims of the invention are fulfilled.
Description
Technical field
The present invention relates to a kind of thermo-stabilizer and preparation method thereof, particularly a kind of cerous hydroxide thermo-stabilizer that is applicable to organo-silicone rubber and preparation method thereof.
Background technology
Compare with General Purpose Rubber; Zylox has excellent thermotolerance, winter hardiness, electrical specification, insulativity and physiology inertia etc., is widely used in fields such as space flight, aviation, electronics, electric, building, machinery, automobile, instrument, chemical industry and medical and health.The outstanding feature of Zylox is its excellent thermotolerance, can be under the temperature about 200 ℃ life-time service, therefore be widely used as the resilient material of high temperature occasion.Along with science and technology development, also increasingly high to the stable on heating requirement of rubber, as the Zylox that is used to apply jet engine, PC board require can be at 250-300 ℃ of following life-time service; The Zylox that is used for the hot air duct of modern supersonic aircraft, high speed car requires the use temperature of ability more than 300 ℃; The Zylox that is used for aerospace industry, its thermotolerance requires higher.Therefore, also need further to improve the thermotolerance of Zylox.
The resistance toheat of improving Zylox improves through the thermotolerance of diverse ways to Zylox from mechanism, has obtained some achievements, conclude get up to have following some: change main chain or side-chain structure; Eliminate the silicon hydroxyl; Add MOX; Add silicone resin; Additive method is as adding the thermal property that oxidation inhibitor such as a spot of diamino-pyrene, quinhydrones or diamino-anthraquinone can improve Zylox in Zylox.Carried out extensive studies with regard to high-temperature-resisting silicon rubber both at home and abroad, as introducing structures such as arylene or aryl oxide support at the Zylox main chain, but this method cost is higher, is mainly used in special dimension.
In Zylox, add heat-resisting additive; Like red oxide of iron, cerium oxide, hexaphenyl ring three silazane etc.; Can prevent the crosslinked and backbone cyclized degraded of ZGK 5 oxide side chain, thereby reach the purpose that improves the silicon rubber heat-resisting performance, this method is a kind of method relatively more commonly used at present.Like SnO
2, Fe
2O
3, Fe (OH)
3, CeO
2Deng the thermo-oxidative stability that can improve Zylox, and SnO
2/ Fe
2O
3Mixture has synergy.Iron copper oxide complex also can improve the thermostability of Zylox, but receives Influence of Temperature, can suppress the thermooxidative degradation of Zylox in the certain temperature range, when surpassing this TR, can quicken the oxidative degradation of Zylox, but no matter be SnO
2, Fe
2O
3, CuO
2Deng adding, can influence the color of Zylox, unfavorable to preparing light Zylox.
It is poor that present thermo-stabilizer ubiquity improves the durability performance of Zylox, and can influence the color of Zylox.
The Chinese patent publication number is that the patent of invention of CN101519506A discloses a kind of high-performance rare earth thermal stabilizer and preparation method thereof, and this thermo-stabilizer is by binary organic acid or its an alkali metal salt and rare earth chemistry thing synthetic binary organic acid rare-earth salts.
The Chinese patent publication number is that the patent of invention of CN102351889A discloses a kind of ring-type rare earth thermal stabilizer and preparation method thereof, and this thermo-stabilizer is by rare earth nitrate, furans, MALEIC ANHYDRIDE chemosynthesis.
The Chinese patent publication number is the compound method that the patent of invention of CN101200556B discloses a kind of PVC thermal stabilizer dicarboxylic acids rear earth salt; Above patent is rare earth organic salt, and this thermo-stabilizer synthesis technique is complicated, and cost is higher.
The thermo-stabilizer that the foregoing invention patent is announced is the composite thermal stabilizer that contains rare earth, has still had complex process, shortcomings such as thermostable effect difference.
Therefore, need a kind of cerous hydroxide thermo-stabilizer and preparation method thereof especially, solved the problem of above-mentioned existing existence.
Summary of the invention
The object of the present invention is to provide a kind of cerous hydroxide thermo-stabilizer and preparation method thereof, overcome prior art and have above-mentioned problem, satisfy the commercial needs of increasingly stringent, improve the added value of rare earth resources.
To achieve these goals, technical scheme of the present invention is following:
On the one hand, the present invention provides a kind of cerous hydroxide thermo-stabilizer, it is characterized in that, the content of rare earth of said thermo-stabilizer is 90-95%, cerium oxide content (CeO
2/ TREO)>=99.9%, calcination loss is 5-10%, median size D
50Be 0.5-3 μ m.
On the other hand, the present invention provides a kind of preparation method of cerous hydroxide thermo-stabilizer, it is characterized in that, it comprises the steps:
(1) removal of impurities: cerous nitrate is dissolved in pure water, be heated to 70-90 ℃ after, add 30% ydrogen peroxide 50, use ammoniacal liquor to regulate pH value and be 4.0-4.5, through vacuum filtration, cerous nitrate solution that must clear;
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution is added 30% ydrogen peroxide 50, use ammoniacal liquor to regulate the pH value and be 8.5-9, be heated to 70-90 ℃ of insulation 1.5-2h, through the plate press filtration, get the cerous hydroxide filter cake;
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains through dry, pulverizing, is got described cerous hydroxide thermo-stabilizer.
In one embodiment of the invention, in step (1), said cerous nitrate is dissolved in pure water, and the cerous nitrate quality accounts for the 30-40% of the quality summation of cerous nitrate and water.
In one embodiment of the invention, in step (1), the purity of said cerous nitrate is CeO
2/ TREO>=99.9%.
In one embodiment of the invention, in step (1), said ydrogen peroxide 50 add-on accounts for the 10-20% of cerous nitrate quality.
In one embodiment of the invention, in step (1), the concentration of said ammoniacal liquor is 10-15%.
In one embodiment of the invention, in step (2), the add-on of said ydrogen peroxide 50 accounts for the 30-40% of cerous nitrate quality.
In one embodiment of the invention, in step (3), said exsiccant condition is 150-180 ℃ of dry 20-30h.
In one embodiment of the invention, in step (3), the mode of said pulverizing comprises conventional grinding modes such as comminution by gas stream and mechanical disintegration.
Cerous hydroxide thermo-stabilizer of the present invention and preparation method thereof is compared with existing product, uses the silastic product of this cerous hydroxide thermo-stabilizer preparation to have the resistance toheat height, and advantages such as goods good colors realize the object of the invention.
Characteristics of the present invention can consult this case graphic and below better embodiment detailed description and obtain to be well understood to.
Description of drawings
Fig. 1 is the particle size distribution figure of embodiments of the invention 1 gained cerous hydroxide thermo-stabilizer;
Fig. 2 is the particle size distribution figure of embodiments of the invention 2 gained cerous hydroxide thermo-stabilizers;
Fig. 3 is the particle size distribution figure of embodiments of the invention 3 gained cerous hydroxide thermo-stabilizers.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, further set forth the present invention below in conjunction with specific embodiment.
On the one hand, cerous hydroxide thermo-stabilizer of the present invention, the content of rare earth of said thermo-stabilizer are 90-95%, cerium oxide content (CeO
2/ TREO)>=99.9%, calcination loss is 5-10%, median size D
50Be 0.5-3 μ m.
On the other hand, the preparation method of cerous hydroxide thermo-stabilizer of the present invention, it comprises the steps:
(1) removal of impurities: cerous nitrate is dissolved in pure water, be heated to 70-90 ℃ after, add 30% ydrogen peroxide 50, use ammoniacal liquor to regulate pH value and be 4.0-4.5, through vacuum filtration, cerous nitrate solution that must clear;
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution is added 30% ydrogen peroxide 50, use ammoniacal liquor to regulate the pH value and be 8.5-9, be heated to 70-90 ℃ of insulation 1.5-2h, through the plate press filtration, get the cerous hydroxide filter cake;
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains through dry, pulverizing, is got described cerous hydroxide thermo-stabilizer.
In the present invention, in step (1), said cerous nitrate is dissolved in pure water, and the cerous nitrate quality accounts for the 30-40% of the quality summation of cerous nitrate and water; The purity of said cerous nitrate is CeO
2/ TREO>=99.9%; Said ydrogen peroxide 50 add-on accounts for the 10-20% of cerous nitrate quality; The concentration of said ammoniacal liquor is 10-15%.
In step (2), the add-on of said ydrogen peroxide 50 accounts for the 30-40% of cerous nitrate quality.
In step (3), said exsiccant condition is 150-180 ℃ of dry 20-30h; The mode of said pulverizing comprises conventional grinding modes such as comminution by gas stream and mechanical disintegration.
(1) removal of impurities: with 300kg cerous nitrate (CeO
2/ TREO>=99.9%) be dissolved in the 700kg pure water, be heated to 70 ℃ after, add 30% ydrogen peroxide 50, using 10% ammoniacal liquor to regulate the pH value is 4.0.Through vacuum filtration, get the cerous nitrate solution of clear.
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution was added 30% ydrogen peroxide 50 90kg, using 10% ammoniacal liquor to regulate the pH value was 8.5, was heated to 70 ℃ of insulation 2h, through the plate press filtration, got the cerous hydroxide filter cake.
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains behind 150 ℃ of dry 30h, through comminution by gas stream, is got described cerous hydroxide thermo-stabilizer.
In the cerous hydroxide thermo-stabilizer that makes, total amount of rare earth is 95%, cerium oxide content (CeO
2/ TREO) be 99.98%, igloss weightlessness is 5%, median size D
50Be 1.19 μ m.(referring to Fig. 1)
(1) removal of impurities: with 400kg cerous nitrate (CeO
2/ TREO>=99.9%) be dissolved in the 600kg pure water, be heated to 90 ℃ after, add 30% ydrogen peroxide 50, using 15% ammoniacal liquor to regulate the pH value is 4.5.Through vacuum filtration, get the cerous nitrate solution of clear.
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution was added 30% ydrogen peroxide 50 120kg, using 15% ammoniacal liquor to regulate the pH value was 9, was heated to 90 ℃ of insulation 1.5h, through the plate press filtration, got the cerous hydroxide filter cake.
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains behind 180 ℃ of dry 20h, through comminution by gas stream, is got described cerous hydroxide thermo-stabilizer.
In the cerous hydroxide thermo-stabilizer that makes, total amount of rare earth is 95%, cerium oxide content (CeO
2/ TREO) be 99.95%, igloss weightlessness is 5.4%, median size D
50Be 0.5 μ m.(referring to Fig. 2)
Embodiment 3
(1) removal of impurities: with 350kg cerous nitrate (CeO
2/ TREO>=99.9%) be dissolved in the 650kg pure water, be heated to 80 ℃ after, add 30% ydrogen peroxide 50, using 12% ammoniacal liquor to regulate the pH value is 4.3.Through vacuum filtration, get the cerous nitrate solution of clear.
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution was added 30% ydrogen peroxide 50 120kg, using 12% ammoniacal liquor to regulate the pH value was 8.7, was heated to 80 ℃ of insulation 1.8h, through the plate press filtration, got the cerous hydroxide filter cake.
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains behind 160 ℃ of dry 25h, through comminution by gas stream, is got described cerous hydroxide thermo-stabilizer.
In the cerous hydroxide thermo-stabilizer that makes, total amount of rare earth is 90%, cerium oxide content (CeO
2/ TREO) be 99.9%, igloss weightlessness is 10%, median size D50 is 3 μ m.(referring to Fig. 3)
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; The present invention is not restricted to the described embodiments; What describe in the foregoing description and the specification sheets is principle of the present invention; The present invention also has various changes and modifications under the prerequisite that does not break away from spirit and scope of the invention, and these variations and improvement all fall in the scope of the present invention that requires protection.The protection domain that the present invention requires is defined by appending claims and equivalent thereof.
Claims (9)
1. a cerous hydroxide thermo-stabilizer is characterized in that, the content of rare earth of said thermo-stabilizer is 90-95%, cerium oxide content (CeO
2/ TREO)>=99.9%, calcination loss is 5-10%, median size D
50Be 0.5-3 μ m.
2. the preparation method of a cerous hydroxide thermo-stabilizer is characterized in that, it comprises the steps:
(1) removal of impurities: cerous nitrate is dissolved in pure water, be heated to 70-90 ℃ after, add 30% ydrogen peroxide 50, use ammoniacal liquor to regulate pH value and be 4.0-4.5, through vacuum filtration, cerous nitrate solution that must clear;
(2) cerous hydroxide is synthetic: after above-mentioned cerous nitrate solution is added 30% ydrogen peroxide 50, use ammoniacal liquor to regulate the pH value and be 8.5-9, be heated to 70-90 ℃ of insulation 1.5-2h, through the plate press filtration, get the cerous hydroxide filter cake;
(3) preparation of thermo-stabilizer: the cerous hydroxide filter cake that obtains through dry, pulverizing, is got described cerous hydroxide thermo-stabilizer.
3. preparation method according to claim 2 is characterized in that, in step (1), said cerous nitrate is dissolved in pure water, and the cerous nitrate quality accounts for the 30-40% of the quality summation of cerous nitrate and water.
4. preparation method according to claim 2 is characterized in that, in step (1), the purity of said cerous nitrate is CeO
2/ TREO>=99.9%.
5. preparation method according to claim 2 is characterized in that, in step (1), said ydrogen peroxide 50 add-on accounts for the 10-20% of cerous nitrate quality.
6. preparation method according to claim 2 is characterized in that, in step (1), the concentration of said ammoniacal liquor is 10-15%.
7. preparation method according to claim 2 is characterized in that, in step (2), the add-on of said ydrogen peroxide 50 accounts for the 30-40% of cerous nitrate quality.
8. preparation method according to claim 2 is characterized in that, in step (3), said exsiccant condition is 150-180 ℃ of dry 20-30h.
9. preparation method according to claim 2 is characterized in that, in step (3), the mode of said pulverizing comprises conventional grinding modes such as comminution by gas stream and mechanical disintegration.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109761259A (en) * | 2019-03-27 | 2019-05-17 | 淄博加华新材料资源有限公司 | A kind of high preparation method at colloidality cerium glue |
| EP4357399A1 (en) | 2022-10-17 | 2024-04-24 | Treibacher Industrie AG | Stabilized polyether-ether-ketone (peek) composition |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109761259A (en) * | 2019-03-27 | 2019-05-17 | 淄博加华新材料资源有限公司 | A kind of high preparation method at colloidality cerium glue |
| CN109761259B (en) * | 2019-03-27 | 2021-04-02 | 淄博加华新材料有限公司 | Preparation method of cerium glue with high gelling property |
| EP4357399A1 (en) | 2022-10-17 | 2024-04-24 | Treibacher Industrie AG | Stabilized polyether-ether-ketone (peek) composition |
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Application publication date: 20121114 |