CN1287967A - Surface preparation of layered dihydroxy composite metal oxide powder - Google Patents
Surface preparation of layered dihydroxy composite metal oxide powder Download PDFInfo
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- CN1287967A CN1287967A CN 99119386 CN99119386A CN1287967A CN 1287967 A CN1287967 A CN 1287967A CN 99119386 CN99119386 CN 99119386 CN 99119386 A CN99119386 A CN 99119386A CN 1287967 A CN1287967 A CN 1287967A
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Abstract
The present invention relates to treatment method of surface modification of laminate bihydroxy clad metal oxide (also called water like talc, or called "LDHs" in short) powder. The modifier is stearic acid, titanate or zirconium aluminate coupling agent, the treatment process in accomplished by adding modifier directly into material pulp while controlling the temperature and mixing time. The invented surface treatment method can obtain surface modification during the preparation of LDHs, which the particles are not aggregated, so that it can prevent the aggregation of particles, simplify the production process, shorten the production period, reduce product cost, reduce energy consumption and equipment investment and avoid environmental pollution.
Description
The invention relates to a surface treatment method of anionic layered inorganic crystal material powder, in particular to a surface treatment method of dihydroxy composite metal oxide powder.
The dihydroxy composite metal oxide is an anionic layered inorganic crystal material, and the chemical composition of the dihydroxy composite metal oxide is generally as follows: wherein M (II) is a divalent metal ion, M (III) is a trivalent metal ion, An-Is n-valent anion, abbreviated as LDHs. It has a layered structure, the framework of the laminate has positive charges, and the ions with opposite charges between layers are balanced with the positive charges, so that the whole structure is electrically neutral. The interlayer anions are exchangeable, and the interlayer spacing shows a specification according to the difference of the interlayer ion sizeThe regularity changes. The chemical composition, the variety and the quantity of ions between layers, the interlayer spacing and the like of the laminated plate can be changed according to design requirements, so that the laminated plate shows different and diversified physical and chemical properties, can be used as a catalytic material, an adsorption and ion exchange material, an infrared absorption material, an ultraviolet barrier material, a flame retardant material, a sterilization material, a medical material and the like, and is widely applied to the fields of rubber, plastics, coatings and the like.
At present, the surface modification of inorganic powder at home and abroad is generally carried out by adopting dry method surface treatment, generally adding the inorganic powder into a high-speed mixer, adding a coupling agent diluted by an organic solvent under high-speed stirring, heating and fully stirring, and although the surface modification method can achieve the expected effect, the following problems exist: (1) the production process is complex; (2) the surface treatment is not uniform enough, and the particles are easy to agglomerate again; (3) the modification process has large dust and environmental pollution; (4) high energy consumption, high investmentof the used modification equipment and high production cost due to the consumption of the organic solvent.
The purpose of the invention is as follows: the surface treatment method of the layered double-hydroxyl composite metal oxide powder is provided, so that LDHs can be subjected to surface treatment in the preparation process, and particles can be subjected to surface modification before aggregation, so that the purposes of avoiding particle aggregation, simplifying the production process, shortening the production period, reducing the product cost, reducing the production energy consumption and the production equipment investment and avoiding environmental pollution are achieved.
The key points of the invention are as follows: a surface treatment method of layered double-hydroxyl composite metal oxide powder is provided, wherein the modifier is selected from any one or combination of the following substances: stearic acid, chelating titanate coupling agent, coordination titanate coupling agent and zirconium aluminate coupling agent. Considering the factors of raw material price, technological process and the like, the modifier is only selected from a single substance in the substance group.
The specific treatment process comprises the following steps: adding the modifier into the prepared slurry of the layered double-hydroxide radical composite metal oxide, stirring and reacting for 15-60 minutes at 30-90 ℃ to ensure that the layered double-hydroxide radical composite metal oxide particles are completely coated by the modifier, and then filtering and drying to obtain the surface modified material.
The slurry of the layered double hydroxide composite metal oxide may be a slurry of a layered double hydroxide composite metal oxide prepared by a different method.
The modifier is used in 0.1-3.0 wt% of the laminated dihydroxy composite metal oxide. The surface treatment is preferably carried out at 70 to 90 ℃.
Since the smaller the particle, the larger the specific surface area, the more the modifier is used, and therefore when the particle size of the layered double hydroxide composite metal oxide is from 1.0 to 10. mu.m, the modifier is preferably used in an amount of from 0.1 to 1.0% by weight based on the layered double hydroxide composite metal oxide; when the particle size of the layered double hydroxide composite metal oxide is 0.1 to 1.0. mu.m, the modifier is preferably used in an amount of 1.0 to 3.0% by weight based on the layered double hydroxide composite metal oxide.
The surface treatment method of the layered double-hydroxy composite metal oxide powder provided by the invention can be used for the surface treatment of the following layered double-hydroxy composite metal oxides:
according to the surface treatment method of the layered double-hydroxy composite metal oxide powder, provided by the invention, the material slurry is treated by using the modifiers such as stearic acid, chelating type titanate coupling agent, coordination type titanate coupling agent or zirconium aluminate coupling agent, so that the layered double-hydroxy composite metal oxide particles are subjected to surface modification when not being aggregated, the integration of powder preparation and modification is realized, the aggregation of the particles is effectively avoided, and the powder is uniformly treated. The method has the advantages of greatly simplified production process, equipment investment saving, short treatment time, no use of organic solvent and no environmental pollution. The surface activation index of the layered dihydroxy composite metal oxide powder treated by the method is 0.85-1.0 (the activation index H = the weight of the floating part of the sample in water/total weight of the sample), and when the layered dihydroxy composite metal oxide powder is applied to a PE film, the tensile strength is 27/28 (longitudinal/transverse), the right-angle tear strength is 115/120 (longitudinal/transverse), and a good surface modification effect is achieved.
The invention is further described with reference to the following examples:
example 1:
(the particle size of the layered double hydroxide composite metal oxide is 0.1 to 1.0. mu.m)
The material slurry comprises the following components in parts by weight:
20 parts of Mg/Al LDHs paste (the water content is 70-80 percent)
80 portions of water
NDZ-311 (trade mark of chelating titanate coupling agent) 0.10 part
Adding the materials into a reaction kettle, heating to 85 ℃, stirring for reaction for 20 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activation index was 0.95.
Example 2:
(the particle size of the layered double hydroxide composite metal oxide is 0.1 to 1.0. mu.m)
The material slurry comprises the following components in parts by weight:
30 parts of Zn/Al LDHs paste (water content is 70-80%)
80 portions of water
0.08 portion of TC-201 (a commercial product brand, belonging to chelate type titanate coupling agent)
Adding the materials into a reaction kettle, heating to 40 ℃, stirring for reaction for 45 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activation index was 1.0.
Example 3:
(the particle size of the layered double hydroxide composite metal oxide is 0.1 to 1.0. mu.m)
The material slurry comprises the following components in parts by weight:
25 parts of Ca/Al LDHs paste (water content is 70-80%)
75 portions of water
Stearic acid 0.14 part
Adding the materials into a reaction kettle, heating to 75 ℃, stirring for reaction for 20 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activation index was 1.0.
Example 4:
(the particle size of the layered double hydroxide composite metal oxide is 1.0 to 10.0. mu.m)
The material slurry comprises the following components in parts by weight:
20 parts of Mg, Zn/Al LDHs paste (water content is 70-80%)
90 portions of water
0.01 part of NDZ-401 (a commercial product brand belonging to a coordination type titanate coupling agent)
Adding the materials into a reaction kettle, heating to 85 ℃, stirring for reaction for 25 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activation index was 0.90.
Example 5:
(the particle size of the layered double-hydroxyl composite metal oxide is 1.0-10.0 mu m) material slurry comprises the following components in parts by weight:
30 parts of Zn, Ni/Al LDHs paste (water content is 70-80%)
80 portions of water
0.04 portion of TC-WT (a commercial product brand, belonging to chelate type titanate coupling agent)
Adding the materials into a reaction kettle, heating to 80 ℃, stirring for reaction for 15 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activity index was 1.0.
Example 6:
(the particle size of the layered double hydroxide composite metal oxide is 1.0 to 10.0. mu.m)
The material slurry comprises the following components in parts by weight:
20 parts of Ca, Ni/Al LDHs paste (water content is 70-80%)
80 portions of water
0.02 portion of TC-301 (a commercial product brand belonging to a zircoaluminate coupling agent)
Adding the materials into a reaction kettle, heating to 85 ℃, stirring for reaction for 25 minutes, and then filtering and drying the reaction mixture to obtain the modified product. The activation index was 0.90.
Example 7:
(the particle size of the layered double hydroxide composite metal oxide is 0.1 to 1.0. mu.m)
The material slurry comprises the following components in parts by weight:
25 parts of Ca/Al LDHs paste (water content is 70-80%)
75 portions of water
Stearic acid 0.10 part
0.01 part of NDZ-401 (a commercial product brand belonging to a coordination type titanate coupling agent)
Adding LDHs filter cake, water and stearic acid into a reaction kettle, heating to 75 ℃, stirring for reaction for 20 minutes, then adding NDZ-401 into the reaction kettle, continuing stirring for reaction for 10 minutes, filtering and drying the reaction mixture, and obtaining the modified product. The activation index was 1.0.
Claims (4)
1. A surface treatment method of layered double-hydroxyl composite metal oxide powder, wherein the modifier is any one or combination of the following substances: stearic acid, chelate type titanate coupling agent, coordination type titanate coupling agent and zircoaluminate coupling agent, and the specific treatment process comprises the following steps: adding the modifier into the slurry of the layered double-hydroxyl composite metal oxide, stirring and reacting at 30-90 ℃, filtering and drying after the layered double-hydroxyl composite metal oxide particles are completely coated by the modifier to obtain the surface modified material.
2. The surface treatment method according to claim 1, wherein: the modifier is any one of the following groups of substances, namely: stearic acid, chelating titanate coupling agent, coordination titanate coupling agent and zirconium aluminate coupling agent, wherein the dosage of the modifier is 0.1-3.0% of the weight of the layered double-hydroxyl composite metal oxide, and the modifier is stirred for reaction for 15-60 minutes.
3. The surface treatment method according to claim 1, wherein: the surface treatment process is carried out at 70-90 deg.C.
4. A surface treatment method according to claim 1, 2 or 3, characterized in that: when the particle size of the layered double-hydroxide radical composite metal oxide is 1.0-10 mu, the dosage of the modifier is 0.1-1.0% of the weight of the layered double-hydroxide radical composite metal oxide; when the particle size of the layered double-hydroxide radical composite metal oxide is 0.1-1.0 mu, the modifier is used in an amount of 1.0-3.0% of the weight of the layered double-hydroxide radical composite metal oxide.
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| CN99119386A CN1099999C (en) | 1999-09-14 | 1999-09-14 | Surface preparation of layered dihydroxy composite metal oxide powder |
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| CN99119386A CN1099999C (en) | 1999-09-14 | 1999-09-14 | Surface preparation of layered dihydroxy composite metal oxide powder |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003037787A1 (en) * | 2001-11-01 | 2003-05-08 | Beijing University Of Chemical Technology | NON-EQUILIBRIUM PROCESS FOR PREPARING A Mg-Al TYPE BISHYDROXY COMPOSITE METAL OXIDE |
| WO2004054361A1 (en) * | 2002-12-13 | 2004-07-01 | Beijing University Of Chemical Technology | A slow-released glyphosate formulation with supermolecular structure and the preparation method thereof |
| CN102453332A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Environment-friendly flame retardant asphalt and preparation method thereof |
| CN101845241B (en) * | 2009-12-31 | 2013-01-09 | 国家复合改性聚合物材料工程技术研究中心 | Preparation method of exfoliated hydrotalcite and application thereof |
| CN103055803A (en) * | 2012-12-20 | 2013-04-24 | 中国科学院生态环境研究中心 | Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent |
| CN103241752A (en) * | 2013-05-29 | 2013-08-14 | 肇庆学院 | Preparation method of surface-modified hydrotalcite |
| CN104592791A (en) * | 2014-12-31 | 2015-05-06 | 安徽恒昊科技有限公司 | Method for preparing silicon treatment talcum powder |
| CN108658507A (en) * | 2018-05-31 | 2018-10-16 | 兰军亚 | A kind of architecture indoor composite functional material and its preparation process |
| CN109137616A (en) * | 2018-07-18 | 2019-01-04 | 内江师范学院 | A kind of paper compounding flame retardant and preparation method thereof |
| CN113355915A (en) * | 2021-06-10 | 2021-09-07 | 安正时尚集团股份有限公司 | Preparation method of breathable fabric with anti-ultraviolet function |
| CN113512337A (en) * | 2021-07-14 | 2021-10-19 | 苏州嘉乐威新材料股份有限公司 | High-adhesion epoxy varnish modified based on load-type corrosion inhibitor and preparation method thereof |
| CN115466549A (en) * | 2022-09-06 | 2022-12-13 | 常州机电职业技术学院 | Ultrathin intumescent fire-proof smoke-suppressing coating based on acrylic polymer emulsion and preparation method thereof |
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| CN100417682C (en) * | 2006-04-13 | 2008-09-10 | 海城金昌滑石粉有限公司 | Use of byproduct rock wool of talcum ore and unqualified waste talcum in plastic |
| CN100437108C (en) * | 2006-10-08 | 2008-11-26 | 浙江工业大学 | Method for detecting surface property of hydrotalcite or hydrotalcite-like substances |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5079203A (en) * | 1990-05-25 | 1992-01-07 | Board Of Trustees Operating Michigan State University | Polyoxometalate intercalated layered double hydroxides |
| CA2082639A1 (en) * | 1990-06-08 | 1991-12-09 | Terence William Turney | Ethylene sorbing substances |
| DE4110835A1 (en) * | 1991-04-04 | 1992-10-08 | Henkel Kgaa | METHOD FOR PRODUCING HYDROPHOBIC DUAL SHEED HYDROXIDE COMPOUNDS |
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1999
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| WO2003037787A1 (en) * | 2001-11-01 | 2003-05-08 | Beijing University Of Chemical Technology | NON-EQUILIBRIUM PROCESS FOR PREPARING A Mg-Al TYPE BISHYDROXY COMPOSITE METAL OXIDE |
| WO2004054361A1 (en) * | 2002-12-13 | 2004-07-01 | Beijing University Of Chemical Technology | A slow-released glyphosate formulation with supermolecular structure and the preparation method thereof |
| CN101845241B (en) * | 2009-12-31 | 2013-01-09 | 国家复合改性聚合物材料工程技术研究中心 | Preparation method of exfoliated hydrotalcite and application thereof |
| CN102453332B (en) * | 2010-10-15 | 2014-05-21 | 中国石油化工股份有限公司 | Environment-friendly flame retardant asphalt and preparation method thereof |
| CN102453332A (en) * | 2010-10-15 | 2012-05-16 | 中国石油化工股份有限公司 | Environment-friendly flame retardant asphalt and preparation method thereof |
| CN103055803A (en) * | 2012-12-20 | 2013-04-24 | 中国科学院生态环境研究中心 | Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent |
| CN103241752A (en) * | 2013-05-29 | 2013-08-14 | 肇庆学院 | Preparation method of surface-modified hydrotalcite |
| CN104592791A (en) * | 2014-12-31 | 2015-05-06 | 安徽恒昊科技有限公司 | Method for preparing silicon treatment talcum powder |
| CN108658507A (en) * | 2018-05-31 | 2018-10-16 | 兰军亚 | A kind of architecture indoor composite functional material and its preparation process |
| CN108658507B (en) * | 2018-05-31 | 2021-04-09 | 赵普平 | Composite functional material for building indoor and preparation process thereof |
| CN109137616A (en) * | 2018-07-18 | 2019-01-04 | 内江师范学院 | A kind of paper compounding flame retardant and preparation method thereof |
| CN113355915A (en) * | 2021-06-10 | 2021-09-07 | 安正时尚集团股份有限公司 | Preparation method of breathable fabric with anti-ultraviolet function |
| CN113512337A (en) * | 2021-07-14 | 2021-10-19 | 苏州嘉乐威新材料股份有限公司 | High-adhesion epoxy varnish modified based on load-type corrosion inhibitor and preparation method thereof |
| CN115466549A (en) * | 2022-09-06 | 2022-12-13 | 常州机电职业技术学院 | Ultrathin intumescent fire-proof smoke-suppressing coating based on acrylic polymer emulsion and preparation method thereof |
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| CN1099999C (en) | 2003-01-29 |
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