CN103241752A - Preparation method of surface-modified hydrotalcite - Google Patents
Preparation method of surface-modified hydrotalcite Download PDFInfo
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- CN103241752A CN103241752A CN2013102060074A CN201310206007A CN103241752A CN 103241752 A CN103241752 A CN 103241752A CN 2013102060074 A CN2013102060074 A CN 2013102060074A CN 201310206007 A CN201310206007 A CN 201310206007A CN 103241752 A CN103241752 A CN 103241752A
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- hydrotalcite
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Abstract
The invention relates to the technical field of surface modification of hydrotalcite and in particular relates to a preparation method of surface-modified hydrotalcite. The preparation method comprises the following steps of: adding a magnesium source, an aluminum source and an alkali source in a molar ratio of (2-6):1:(0.5-27) in a combined manner; adding a surface modifying agent which is 0.1%-5% of the theoretical amount of the hydrotalcite, sufficiently stirring, and carrying out crystallization for 4-20 hours in a hydrothermal reaction kettle within a temperature range of 110-200 DEG C; and washing, filtering and drying to obtain the surface-modified hydrotalcite. The preparation method of the surface-modified hydrotalcite provided by the invention can be used for completing the hydrotalcite synthesis and the surface modification of the hydrotalcite by one step, i.e., completing surface modification in a hydrotalcite hydro-thermal synthesis process, so that the hydrotalcite preparation and the surface modification are integrated, and therefore, the production process is simplified, the production time is saved and the production cost is lowered.
Description
Technical field
The present invention relates to hydrotalcite process for modifying surface field, be specifically related to a kind of preparation method of hydrotalcite of surface modification.
Background technology
Hydrotalcite-based compound (LDHs) is the anion type laminated compound that a class has broad prospect of application, mainly comprises hydrotalcite (HT), houghite (being called for short HTLC) and their intercalation chemistry product pillared hydrotalcite (Pillared LDH).Owing to formed by the metal oxide of two kinds of different price types between the hydrotalcite-based compound laminate, claim layered bi-metal oxide compound (being called for short LDH) again.Typical hydrotalcite molecular formula is Mg
6A
L2(OH)
16CO
34H
2O has the brucite of being similar to [Mg (OH)
2] the regular octahedron structure, adjacent octahedron becomes unit layer by sharing prismatic, is positioned at the Mg on the layer
2+Can be within the specific limits by the Al of similar radius
3+Isomorphous substitution causes the positive charge accumulation on the hydroxyl layer, and these skeleton positive charges are positioned at the negatively charged ion CO of interlayer
3 2-Balance makes entire structure be electric neutrality.At interlayer, some water moleculess exist with crystalline state, can remove under the condition of breakable layer rod structure not.Special chemical structure and crystalline structure, given the performance of a series of excellences of hydrotalcite, as Modulatory character of the Modulatory character of laminate chemical constitution, interlayer anion interchangeability, grain size distribution etc., it is widely used in the fields such as rubber, plastics and coating.
Along with the range of application of hydrotalcite is more and more wider, demand is also increasing.Yet because the hydrotalcite surface has active group-OH, surface energy is big, and it is soft-agglomerated very easily to form the hydrogen bond generation, produces hard aggregation with the condensation of coordinated water molecule, thereby has influenced its dispersiveness in organism matrix.In addition, the affinity of hydrotalcite and organic materials is poor, easily forms " half-cooked " phenomenon when directly or in a large number being filled in the polymkeric substance, causes the mechanical properties decrease of material etc., has limited its widespread use.Hydrotalcite is carried out surface modification, can effectively prevent from reuniting and take place, can improve the consistency of hydrotalcite and polymkeric substance simultaneously, and then enlarge its range of application.At present, the surface modification of hydrotalcite generally adopts the dry powder surface modification, and this method operating procedure complexity is difficult to abundant dispersion to the hydrotalcite of having reunited, and surface modification is also inhomogeneous, and simultaneously, dust is big in the modifying process, easily causes environmental pollution.Someone adds anionic, sodium stearate etc. in the crystallization later stage of coprecipitation method synthetic hydrotalcite, and hydrotalcite is carried out simple organic parcel, and this process is loaded down with trivial details, and modified effect is not ideal enough.Also have the people properties-correcting agent to be joined in the hydrotalcite material slurry that has prepared, control certain temperature and churning time are finished modification, this method production technique relative complex, and the production time is longer.Therefore, all there is certain shortcoming in above-mentioned method of modifying, and production cost is than higher.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of hydrotalcite of surface modification, in the hydrotalcite building-up process, carry out surface modification simultaneously, hydrotalcite surface modification and a synthetic step are finished, thereby simplify production technique greatly, shorten the production cycle, reduce production costs, and can effectively avoid environmental pollution.
The preparation method of the hydrotalcite of surface modification of the present invention may further comprise the steps: in molar ratio for the 2-6:1:0.5-27 combination feeds intake, wherein the amount of alkali source is in the hydroxide radical amount of substance with magnesium source, aluminium source, alkali source; Add the surface-modifying agent of the 0.1%-5% that accounts for gained hydrotalcite theoretical amount simultaneously, wherein the theoretical amount of hydrotalcite is by the hydrotalcite structure general formula: (Mg
2+)
1-x(Al
3+)
x(OH)
2(CO
3 2-)
X/2b.dH
2O calculates; Fully stir down, in 110-200 ℃ of temperature range, in hydrothermal reaction kettle crystallization 4-20 hour, finally by washing, filtration, drying, namely obtain the hydrotalcite of surface modification.
According to preparation method's of the present invention further feature, described magnesium source is to be selected from: at least a in magnesium oxide, magnesium hydroxide, magnesium nitrate, sal epsom, the magnesium chloride.
According to preparation method's of the present invention further feature, described aluminium source is to be selected from: at least a in aluminium hydroxide, aluminum oxide, aluminum nitrate, Tai-Ace S 150, the aluminum chloride.
According to preparation method's of the present invention further feature, described surface-modifying agent is at least a in nonionogenic tenside, titanate coupling agent, the silane coupling agent.Preferably, described nonionogenic tenside is polyoxyethylene-type or polyol-based non-ionic surfactant.Preferably, described titanate coupling agent is corrdination type titanate coupling agent or chelating titanate coupling agent.Preferably, the general formula of described silane coupling agent is Y (CH
2) nSiX, wherein Y is epoxy group(ing), methacryloxy.According to the difference of magnalium feed ratio in the hydrotalcite building-up process, the properties-correcting agent consumption is different.
According to preparation method's of the present invention further feature, described alkali source is to be selected from: at least a in sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, the ammoniacal liquor or can react the compound that generates sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, ammoniacal liquor in building-up process.
The preparation method of the hydrotalcite of surface modification of the present invention, its advantage is: adopt hydrothermal synthesis method, properties-correcting agent and magnesium source, aluminium source, alkali source once feed intake, hydrotalcite is synthetic to carry out simultaneously with surface modification, thereby a step is finished the synthetic and surface modification of hydrotalcite, namely can in the process of hydro-thermal synthetic hydrotalcite, finish surface modification simultaneously, realize the integrated of hydrotalcite preparation and surface modification.Method provided by the present invention is simplified production technique greatly, has avoided environmental pollution, has saved the production time, has significantly reduced production cost.And the surface modification hydrotalcite according to preparation method of the present invention obtains has the following advantages: synthetic hydrotalcite has complete laminate structure, and crystalline phase single, be uniformly dispersed, effectively avoided reunion.The surface active index of hydrotalcite represents that for the 0.9-1.0(degree of activation sample is in the weight/sample gross weight of water float part), be applied among the PVC and can reach effect preferably.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) figure of hydrotalcite after the surface modification.
Fig. 2 is infrared spectra (FTIR) figure of hydrotalcite before and after the surface modification; Among the figure, before A represents modification; After B represents modification.
Fig. 3 is scanning electron microscope (SEM) figure of hydrotalcite before and after the surface modification; Among the figure, before the left figure expression modification; After the right figure expression modification.
Embodiment
Below in conjunction with concrete exemplifying embodiment the present invention is described in more detail and illustrates.
Embodiment 1
Weighing 0.81g magnesium oxide, 0.78g aluminium hydroxide, 1.06g yellow soda ash, the single propylene glycol stearate of 0.08g, a certain amount of water stirs in the 25ml hydrothermal reaction kettle, in 140 ℃ of constant temperature 16h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the surface modification hydrotalcite.Degree of activation is 0.99.
Degree of activation is one of hydrophobic measurement index after the inorganics surface modification, is used for judging inorganics surface coating degree.The mensuration of hydrotalcite degree of activation is with reference to GB/T 19281-2003, and the degree of activation of unmodified hydrotalcite is 0.
The mensuration of embodiment 1 preparation products obtained therefrom.Shown in the XRD figure of Fig. 1, the diffraction peak of product all matches with card JCPDS22-700, and does not have other dephasign diffraction peak to occur, and shows that synthetic product is hydrotalcite, and the structure homogeneous, the degree of crystallinity height.Shown in the FTIR figure of Fig. 2, there are hydroxyl and CO in the product
3 2-, wave number is 3454cm
-1The place is the hydroxyl vibration absorption peak, and wave number is 2922 cm
-1, 2853cm
-1Be respectively unsymmetrically, the symmetrical stretching vibration absorption peak of methylene radical, wave number is 1369cm
-1Be CO
3 2-Vibration absorption peak, wave number are 451cm
-1Be hydrotalcite skeletal vibration charateristic avsorption band.Shown in the SEM figure of Fig. 3, after surface modification, agglomeration be improved significantly.The result shows according to said determination, the hydrotalcite of successful synthetic surface modification.
Embodiment 2
Weighing 4.1g magnesium hydroxide, 1.56g aluminium hydroxide, 2.12g yellow soda ash, 0.32g sodium hydroxide, 0.30g Macrogol 2000, a certain amount of water is in the 25ml hydrothermal reaction kettle, stir, in 120 ℃ of constant temperature 20h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the surface modification hydrotalcite.Degree of activation is 1.0.
Embodiment 3
Weighing magnesium nitrate 15.0g, aluminum nitrate 9.6g, 0.24g titanate coupling agent KR-201 add 50ml water in the 250ml beaker, stirring and dissolving is made into A liquid; Weighing 7.2g sodium hydroxide, 2.12g yellow soda ash add 50ml water in the 100ml beaker, stirring and dissolving, be made into B liquid, then at 100 ℃, under the violent stirring A, B liquid mixed, continue to stir 1h, again slurries are transferred in the reactor, in 130 ℃ of constant temperature 8h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 0.95.
Embodiment 4
Weighing magnesium chloride 5.7g, aluminum chloride 1.3g, 0.24g silane coupling agent HK-560 add 50ml water in the 250ml beaker, stirring and dissolving is made into A liquid; Weighing 9.2g sodium hydroxide, 2.12g yellow soda ash add 50ml water in the 100ml beaker, stirring and dissolving, be made into B liquid, then at 80 ℃, under the violent stirring A, B liquid mixed, continue to stir 1h, again slurries are transferred in the reactor, in 110 ℃ of constant temperature 4h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 0.96.
Embodiment 5
Weighing sal epsom 17.3g, Tai-Ace S 150 4.7g, 0.4g silane coupling agent HK-570 add 50ml water in the 250ml beaker, stirring and dissolving is made into A liquid; Weighing 9.2g sodium hydroxide, 2.12g yellow soda ash add 50ml water in the 100ml beaker, stirring and dissolving, be made into B liquid, then at 90 ℃, under the violent stirring A, B liquid mixed, continue to stir 1h, again slurries are transferred in the reactor, in 140 ℃ of constant temperature 8h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 0.98.
Embodiment 6
Weighing 6.9g magnesium hydroxide, 1.5g aluminum oxide, 3.00g yellow soda ash, the ammoniacal liquor of 1.5ml 28%, 0.10g Macrogol 4000, a certain amount of water adds it in reactor, stirs, in 200 ℃ of constant temperature 8h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 0.92.
Embodiment 7
Weighing 6.00g magnesium oxide, 2.34g aluminium hydroxide, 3.18g yellow soda ash, 0.22g potassium hydroxide, 0.11g this dish-20, a certain amount of water places reactor, stirs, in 130 ℃ of constant temperature 8h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 0.90.
Embodiment 8
Weighing 3.00g magnesium oxide, the 1.53g aluminum oxide, the 2.52g sodium bicarbonate, the 0.21g Tween-60, a certain amount of water places reactor, stirs, in 110 ℃ of constant temperature 18h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the hydrotalcite of surface modification.Degree of activation is 1.0.
Embodiment 9
Weighing 2.42g magnesium oxide, 1.56g aluminium hydroxide, 2.12g yellow soda ash, the ammoniacal liquor of 1ml 28%, 0.006g single propylene glycol stearate, a certain amount of water in the 25ml hydrothermal reaction kettle, stirs, in 180 ℃ of constant temperature 10h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the surface modification hydrotalcite.Degree of activation is 0.90.
Weighing 3.5g magnesium hydroxide, 1.0g aluminum oxide, 2.12g yellow soda ash, 0.45g sodium hydroxide, 0.30g single propylene glycol stearate, a certain amount of water in the 25ml hydrothermal reaction kettle, stirs, in 110 ℃ of constant temperature 20h, cooling back suction filtration, washing, 90 ℃ of dry 12h namely get the surface modification hydrotalcite.Degree of activation is 0.99.
Above-mentioned these embodiment only are used for illustrating content of the present invention, by these embodiment, those skilled in the art should know, preparation method for the hydrotalcite of surface modification of the present invention, described magnesium source can be selected from: magnesium oxide, magnesium hydroxide, magnesium nitrate, sal epsom, magnesium chloride, perhaps their analogue; Described aluminium source can be selected from: aluminium hydroxide, aluminum oxide, aluminum nitrate, Tai-Ace S 150 or aluminum chloride, perhaps their analogue.Described surface-modifying agent can be selected from: nonionogenic tenside, for example polyoxyethylene-type or polyol-based non-ionic surfactant; Titanate coupling agent, for example corrdination type titanate coupling agent or chelating titanate coupling agent; Silane coupling agent, for example general formula is Y (CH
2) silane coupling agent of nSiX, wherein Y is epoxy group(ing), methacryloxy.Described alkali source can be selected from: at least a in sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, the ammoniacal liquor or can react the compound that generates sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, ammoniacal liquor in building-up process.
Claims (8)
1. the preparation method of the hydrotalcite of a surface modification is characterized in that may further comprise the steps:
In molar ratio for the 2-6:1:0.5-27 combination feeds intake, wherein the amount of alkali source is in the hydroxide radical amount of substance with magnesium source, aluminium source, alkali source;
Add the surface-modifying agent of the 0.1%-5% that accounts for gained hydrotalcite theoretical amount simultaneously, wherein the theoretical amount of hydrotalcite is by the hydrotalcite structure general formula: (Mg
2+)
1-x(Al
3+)
x(OH)
2(CO
3 2-)
X/2b.dH
2O calculates;
Fully stir down, in 110-200 ℃ of temperature range, in hydrothermal reaction kettle crystallization 4-20 hour, finally by washing, filtration, drying, namely obtain the hydrotalcite of surface modification.
2. preparation method according to claim 1, it is characterized in that: described magnesium source is to be selected from: at least a in magnesium oxide, magnesium hydroxide, magnesium nitrate, sal epsom, the magnesium chloride.
3. preparation method according to claim 1, it is characterized in that: described aluminium source is to be selected from: at least a in aluminium hydroxide, aluminum oxide, aluminum nitrate, Tai-Ace S 150, the aluminum chloride.
4. preparation method according to claim 1 is characterized in that: described surface-modifying agent is at least a in nonionogenic tenside, titanate coupling agent, the silane coupling agent.
5. preparation method according to claim 4, it is characterized in that: described nonionogenic tenside is polyoxyethylene-type or polyol-based non-ionic surfactant.
6. preparation method according to claim 4, it is characterized in that: described titanate coupling agent is corrdination type titanate coupling agent or chelating titanate coupling agent.
7. preparation method according to claim 4, it is characterized in that: the general formula of described silane coupling agent is Y (CH
2) nSiX, wherein Y is epoxy group(ing), methacryloxy.
8. preparation method according to claim 1, it is characterized in that: described alkali source is to be selected from: at least a in sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, the ammoniacal liquor or can react the compound that generates sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate, ammoniacal liquor in building-up process.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710649A (en) * | 2015-03-24 | 2015-06-17 | 宁波高新区零零七工业设计有限公司 | Method for preparing hydrotalcite heat stabilizer |
| CN104893136A (en) * | 2014-03-03 | 2015-09-09 | 南通艾德旺化工有限公司 | Preparation method for modified composite magnesium aluminum hydrotalcite heat stabilizer |
| CN107190255A (en) * | 2017-04-11 | 2017-09-22 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN108623843A (en) * | 2018-03-23 | 2018-10-09 | 邵阳天堂助剂化工有限公司 | Modified hydrotalcite and its clean method for preparing for PVC heat stabilizer |
| CN109989294A (en) * | 2019-03-29 | 2019-07-09 | 潍坊科技学院 | A kind of preparation method of organically-modified hydrotalcite Flame Retardant in Paper |
| CN110183999A (en) * | 2019-05-30 | 2019-08-30 | 刘丹 | A kind of preparation method of ageing-resistant glue spraying |
| CN110395753A (en) * | 2019-07-06 | 2019-11-01 | 王志胜 | A kind of preparation method of epigranular high stable houghite |
| CN110496589A (en) * | 2019-08-27 | 2019-11-26 | 西安交通大学 | A kind of hydrotalcite and preparation method thereof and application of the hydrotalcite in adsorbed water body in PFOS pollutant |
| CN110713638A (en) * | 2018-07-11 | 2020-01-21 | 北京化工大学 | Hydrotalcite/epoxy natural rubber/styrene butadiene rubber composite material and preparation method thereof |
| CN113318702A (en) * | 2021-04-09 | 2021-08-31 | 吉林化工学院 | Preparation and application of modified bimetal oxide |
| CN114634783A (en) * | 2022-04-13 | 2022-06-17 | 广州慧能新材料科技有限公司 | Halogen-free flame-retardant high-temperature-resistant epoxy resin sealant and preparation method thereof |
| CN115536907A (en) * | 2022-09-15 | 2022-12-30 | 呈和科技股份有限公司 | Special hydrotalcite additive for agricultural film and application thereof |
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Cited By (16)
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| CN104893136A (en) * | 2014-03-03 | 2015-09-09 | 南通艾德旺化工有限公司 | Preparation method for modified composite magnesium aluminum hydrotalcite heat stabilizer |
| CN104710649A (en) * | 2015-03-24 | 2015-06-17 | 宁波高新区零零七工业设计有限公司 | Method for preparing hydrotalcite heat stabilizer |
| CN107190255A (en) * | 2017-04-11 | 2017-09-22 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN107190255B (en) * | 2017-04-11 | 2019-04-16 | 中国科学院上海硅酸盐研究所 | A kind of super-hydrophobic magnesium or magnesium alloy materials and its preparation method and application |
| CN108623843A (en) * | 2018-03-23 | 2018-10-09 | 邵阳天堂助剂化工有限公司 | Modified hydrotalcite and its clean method for preparing for PVC heat stabilizer |
| CN110713638B (en) * | 2018-07-11 | 2020-12-11 | 北京化工大学 | Hydrotalcite/epoxy natural rubber/styrene butadiene rubber composite material and preparation method thereof |
| CN110713638A (en) * | 2018-07-11 | 2020-01-21 | 北京化工大学 | Hydrotalcite/epoxy natural rubber/styrene butadiene rubber composite material and preparation method thereof |
| CN109989294A (en) * | 2019-03-29 | 2019-07-09 | 潍坊科技学院 | A kind of preparation method of organically-modified hydrotalcite Flame Retardant in Paper |
| CN110183999A (en) * | 2019-05-30 | 2019-08-30 | 刘丹 | A kind of preparation method of ageing-resistant glue spraying |
| CN110395753A (en) * | 2019-07-06 | 2019-11-01 | 王志胜 | A kind of preparation method of epigranular high stable houghite |
| CN110496589A (en) * | 2019-08-27 | 2019-11-26 | 西安交通大学 | A kind of hydrotalcite and preparation method thereof and application of the hydrotalcite in adsorbed water body in PFOS pollutant |
| CN110496589B (en) * | 2019-08-27 | 2020-11-10 | 西安交通大学 | Hydrotalcite, preparation method thereof and application of hydrotalcite in PFOS (Perfluorooctane sulfonate) pollutant adsorption in water body |
| CN113318702A (en) * | 2021-04-09 | 2021-08-31 | 吉林化工学院 | Preparation and application of modified bimetal oxide |
| CN114634783A (en) * | 2022-04-13 | 2022-06-17 | 广州慧能新材料科技有限公司 | Halogen-free flame-retardant high-temperature-resistant epoxy resin sealant and preparation method thereof |
| CN114634783B (en) * | 2022-04-13 | 2023-11-10 | 醴陵市京渌新材料有限公司 | Halogen-free flame-retardant high-temperature-resistant epoxy resin sealant and preparation method thereof |
| CN115536907A (en) * | 2022-09-15 | 2022-12-30 | 呈和科技股份有限公司 | Special hydrotalcite additive for agricultural film and application thereof |
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Application publication date: 20130814 |