CN1252161C - Organic composite rectorite and preparation process thereof - Google Patents
Organic composite rectorite and preparation process thereof Download PDFInfo
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- CN1252161C CN1252161C CN 02115758 CN02115758A CN1252161C CN 1252161 C CN1252161 C CN 1252161C CN 02115758 CN02115758 CN 02115758 CN 02115758 A CN02115758 A CN 02115758A CN 1252161 C CN1252161 C CN 1252161C
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Abstract
The present invention relates to organic composite rectorite basically prepared (by weight) from 1 to 100 portions of rectorite, 0.2 to 30 portions of organic intercalation agent and 0.01 to 5.0 portions of protonating agent. The preparation method of the organic composite rectorite comprises: the rectorite is dispersed in water to form a stable suspension; after the organic intercalation agent and the protonating agent are added into the water and stirred to form a solution, the solution is added into the suspension; the obtained mixture is stirred at high speed, filtered, washed, dried and pulverized to obtain the needed organic composite rectorite. In the present invention, the interlamellar spacing of the rectorite is enlarged 4 nanometers more or less after the rectorite is modified by the organic intercalation agent, and simultaneously, the hydrophilic surface of the rectorite is converted into a lipophilic surface so that the rectorite can be dispersed in organic solvents, such as toluene, ethanol, propanone, etc.; the rectorite acting on a monomer melt or a polymer melt can be stripped into structural lamellas of a nanometer scale in a polymerization process or a mixing process, and the structural lamellas are homogeneously dispersed into a polymeric matrix to obtain a polymeric nanometer composite material.
Description
Technical field
The present invention relates to organic composite rectorite and preparation method thereof.
Background technology
Rectorite leng is the important layered silicate material of a class, be 1: 1 regular interbed mineral of dioctahedron mica layer and dioctahedron smectite layer, its crystalline structure alternately is stacked to regularly by class mica unit layer and class smectite unit layer, about about 2.2～2.4 nanometers of interlamellar spacing, about 2.2 nanometers of the interlamellar spacing of sodium rectorite leng.If with itself and monomer or polymer melt effect, in polymerization or mixing process, peel off into the structure lamella of nanoscale, evenly spread in the polymeric matrix, prepared nano composite polymer/laminated silicate material has the incomparable advantage of conventional matrix material, as mechanics, the thermal property of excellence, and barrier properties for gases etc.Problem is that above-mentioned rectorite leng surface is wetting ability, is difficult to make above-mentioned polymer nanocomposites with the consistency difference of polymkeric substance.
Summary of the invention
The present invention be exactly at the problems referred to above provide a kind of be used to prepare nano composite polymer/laminated silicate material, the surface has hydrophobic oil loving organic composite rectorite and preparation method thereof.
Technical scheme provided by the invention is: a kind of organic composite rectorite, it basic composition is: 1～100 part of rectorite leng, 0.2～30 part of organic intercalation agent, 0.01～5.0 part of protonating agent more than are parts by weight.
Above-mentioned rectorite leng raw material is the layered silicate that contains 80～95% rectorite lengs, and its particle diameter is 20～80 microns, and the cationic exchange total amount is 13～38 milligramequivalents/100 grams.
Above-mentioned intercalator is that chain alkyl (carbonatoms is 12～18) quaternary ammonium salt, nylon salt or carbonatoms are 6～12 amino acid.
Above-mentioned protonating agent is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid.
The present invention also provides the preparation method of above-mentioned organic composite rectorite, and 1～100 part of rectorite leng is dispersed in 15～3000 parts of water, and high-speed stirring is until forming steady suspension; In addition 0.2～30 part of organic intercalation agent, protonating agent are joined in 5～1000 parts of water for 0.01～5.0 part, after 60～80 ℃ stirring forms solution down, join in the above-mentioned rectorite leng suspension, the gained mixture is high-speed stirring 3～4 hours again, filter, washing, dry, pulverize and promptly get required organic composite rectorite; Above umber is parts by weight.
The present invention with rectorite leng after the organic intercalation modification, because organic intercalation agent is arranged at interlayer regularly, its belt length alkyl group has certain sterically hindered, interlamellar spacing is increased to about 4 nanometers, the surface is changed lipophilicity into by wetting ability simultaneously, can be scattered in toluene, ethanol, the acetone and other organic solvent; With monomer or polymer melt effect, in polymerization or mixing process, can peel off into the structure lamella of nanoscale and evenly spread in the polymeric matrix, make polymer nanocomposites.
Embodiment
Embodiment 1: a kind of organic composite rectorite, it basic composition is: 2 parts of rectorite lengs, 0.2 part of organic intercalation agent, 0.02 part of protonating agent more than are parts by weight.
Embodiment 2: a kind of organic composite rectorite, it basic composition is: 100 parts of rectorite lengs, 10 parts of organic intercalation agents, 2 parts of protonating agents more than are parts by weight.
Embodiment 3: a kind of organic composite rectorite, it basic composition is: 50 parts of rectorite lengs, 25 parts of organic intercalation agents, 5.0 parts of protonating agents more than are parts by weight.
Embodiment 4: a kind of organic composite rectorite, it basic composition is: 20 parts of rectorite lengs, 1 part of organic intercalation agent, 0.03 part of protonating agent more than are parts by weight.
Embodiment 5: a kind of organic composite rectorite, it basic composition is: 60 parts of rectorite lengs, 2 parts of organic intercalation agents, 0.5 part of protonating agent more than are parts by weight.
Above-mentioned rectorite leng raw material is the layered silicate that contains 80～95% rectorite lengs, and its particle diameter is 20～80 microns, and the cationic exchange total amount is 13～38 milligramequivalents/100 grams.
Above-mentioned intercalator is that chain alkyl (carbonatoms is 12～18) quaternary ammonium salt, nylon salt or carbonatoms are 6～12 amino acid.
Above-mentioned protonating agent is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid.
The preparation method of organic composite rectorite among the embodiment 1～5 is dispersed in the rectorite leng of corresponding content in 15～3000 parts of water, and high-speed stirring is until forming steady suspension; Organic intercalation agent, protonating agent with corresponding content joins in 5～1000 parts of water in addition, be heated to 60～80 ℃, join in the above-mentioned rectorite leng suspension after stirring formation solution, the gained mixture is high-speed stirring 3～4 hours again, filter, washing, dry, pulverize and promptly get required organic composite rectorite.
Embodiment 6: get 5 gram purity greater than 90% sodium rectorite leng, add 400 milliliters in water, the even outstanding turbid system that must be stable of dispersed with stirring, other gets 2 gram hexadecylamines, adds 400 milliliters in water, 0.3 milliliter of hydrochloric acid, be heated to 80 ℃, be stirred to dissolving fully, form homogeneous solution.Alkylammonium salt solution is joined in the above-mentioned suspension, continue to stir four hours, decompress filter, massive laundering, drying is pulverized and is promptly got required organic composite rectorite.Observe through X-ray diffraction, find its d
001Interplanar distance increases to 3.8 nanometers by 2.2 nanometers of sodium rectorite leng; And composite rectorite changes hydrophobic oleophylic into by original wetting ability, can be scattered in toluene, ethanol, the acetone and other organic solvent.
Embodiment 7: get 80 gram purity greater than 90% sodium rectorite leng, add 2000 milliliters in water, the even outstanding turbid system that must be stable of dispersed with stirring, other gets 25 gram cetyl trimethyl amine, adds 800 milliliters in water, 3.0 milliliters of hydrochloric acid, be heated to 80 ℃, be stirred to dissolving fully, form homogeneous solution.Alkylammonium salt solution is joined in the above-mentioned suspension, continue to stir four hours, decompress filter, massive laundering, drying is pulverized and is promptly got required organic composite rectorite.Observe through X-ray diffraction, find its d
001Interplanar distance increases to 4.1 nanometers by 2.2 nanometers of sodium rectorite leng; And composite rectorite changes hydrophobic oleophylic into by original wetting ability, can be scattered in toluene, ethanol, the acetone and other organic solvent.
Hexadecylamine among the embodiment 6,7, cetyl trimethyl amine can be that 6～12 amino acid or carbonatoms are 12～18 to be that other long chain alkyl ammonium salt replaces with nylon salt, carbonatoms; Protonating agent hydrochloric acid can use sulfuric acid, nitric acid, phosphoric acid or acetic acid to replace, and also can make required organic composite rectorite as method.
Claims (5)
1. organic composite rectorite, it basic composition is: 1～100 part of rectorite leng, 0.2～30 part of organic intercalation agent, 0.01～5.0 part of protonating agent more than are parts by weight.
2. according to the described organic composite rectorite of claim 1, it is characterized in that: described rectorite leng is the layered silicate that contains 80～95% rectorite lengs, and its particle diameter is 20～80 microns, and the cationic exchange total amount is 13～38 milligramequivalents/100 grams.
3. according to claim 1 or 2 described organic composite rectorites, it is characterized in that: intercalator is that long chain alkyl ammonium salt, nylon salt or carbonatoms are 6～12 amino acid.
4. according to claim 1 or 2 described organic composite rectorites, it is characterized in that: protonating agent is hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid or acetic acid.
5. the preparation method of the described organic composite rectorite of claim 1 is dispersed in 1～100 part of rectorite leng in 15～3000 parts of water, and high-speed stirring is until forming steady suspension; In addition 0.2～30 part of organic intercalation agent, protonating agent are joined in 5～1000 parts of water for 0.01～5.0 part, after 60～80 ℃ stirring forms solution down, join in the above-mentioned rectorite leng suspension, the gained mixture is high-speed stirring 3～4 hours again, filter, washing, dry, pulverize and promptly get required organic composite rectorite; Above umber is parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02115758 CN1252161C (en) | 2002-04-25 | 2002-04-25 | Organic composite rectorite and preparation process thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02115758 CN1252161C (en) | 2002-04-25 | 2002-04-25 | Organic composite rectorite and preparation process thereof |
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| CN1385470A CN1385470A (en) | 2002-12-18 |
| CN1252161C true CN1252161C (en) | 2006-04-19 |
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| CN 02115758 Expired - Fee Related CN1252161C (en) | 2002-04-25 | 2002-04-25 | Organic composite rectorite and preparation process thereof |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100413923C (en) * | 2003-06-11 | 2008-08-27 | 武汉大学 | Nano composite material of epoxy resin and its preparing method |
| CN100451060C (en) * | 2005-12-16 | 2009-01-14 | 武汉大学 | Chitosan/rectorite nano composite materials and method for preparing the same |
| CN103122138B (en) * | 2013-01-22 | 2016-01-20 | 安徽华津电缆集团有限公司 | Power cable TPU/SEBS thermoplastic elastomer Insulating Material and Preparation Method |
| CN103232721B (en) * | 2013-04-27 | 2016-12-28 | 衡阳建祥新材料有限公司 | A kind of waste or used plastics produces, with flyash, the method that microcrystalline carbon moulds sheet material |
| CN103525007A (en) * | 2013-09-09 | 2014-01-22 | 宝应县瑞材电工材料有限公司 | Method for preparing rectorite-modified epoxy resin/glass fiber composite material |
| CN105753004B (en) * | 2016-01-26 | 2017-12-26 | 武汉华矿胶体化学有限公司 | A kind of organic clay and its production method of big interplanar distance |
| CN106957492A (en) * | 2017-04-07 | 2017-07-18 | 安徽省无为县经纬电缆附件有限公司 | A kind of heating cable is with wear-resisting tear-resistant protective cover material |
| CN115893437A (en) * | 2022-10-10 | 2023-04-04 | 中国科学技术大学 | Layered silicate clay mineral nanosheet and preparation method thereof |
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