CN103819949A - Surface modification method for inorganic powder - Google Patents
Surface modification method for inorganic powder Download PDFInfo
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- CN103819949A CN103819949A CN201410090140.2A CN201410090140A CN103819949A CN 103819949 A CN103819949 A CN 103819949A CN 201410090140 A CN201410090140 A CN 201410090140A CN 103819949 A CN103819949 A CN 103819949A
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Abstract
The invention discloses a surface modification method for inorganic powder. The method comprises the following steps: 100 parts of inorganic powder, 1-6 parts of 20-100 meshes of ethylene-vinyl alcohol copolymer and 5-30 parts of glycerinum are conducted activating treatment under the temperature of 165-200 DEG for 10-30 min to obtain surface modified inorganic powder. According to the invention, the consistency and dispersibility of the inorganic powder in polymer matrixes can be effectively improved, the surface modification method is simple, the requirements on equipment are low, and popularization and application are facilitated, and the surface modification method has obvious economic and social benefits.
Description
Technical field
The invention belongs to the process for modifying surface field of inorganic powder, relate to a kind of preparation method through ethylene-vinyl alcohol copolymer surface-modified inorganic powder.Be to use ethylene-vinyl alcohol copolymer modified inorganic powder specifically, make its surface become oil loving method of modifying from wetting ability.
Background technology
Inorganic powder is as calcium carbonate, calcium oxide, calcium hydroxide, aluminium hydroxide, aluminum oxide, magnesium hydroxide, magnesiumcarbonate, magnesium oxide, brucite, rhombspar, calcite, slag magnesiumcarbonate, Sodium Aluminium Carbonate Basic, wollastonite, kaolin, clay, mica, talcum powder, silicon-dioxide, titanium dioxide, glass microballon, marble, chalk, Wingdale, barium sulfate, nepheline, potassium felspar sand, albite, graphite, carbon black, zinc oxide, the mineral such as zinc carbonate are at plastics, rubber, synthon, coating, in the Macromolecular materials industries such as binding agent, have a wide range of applications, there is the macromolecular material of reduction and goods cost, give macromolecular material functional, the effect of the new purposes of exploitation macromolecular material.Therefore the application of inorganic powder in macromolecular material is subject to the attention of researcher and vast processing of high molecular material manufacturer always deeply.Particularly after 2003, along with producing synthetic resins starting material---the big bulge in price of oil, and the growing interest of the environmental pollution that macromolecular material is caused, derive from nature, again can return in nature, have good environment Harmony, and the inorganic powder that can reduce macromolecular material usage quantity be day by day subject to people's great attention.
The surface properties of inorganic powder is generally wetting ability, and has larger difference between organic polymer material matrix.Organic polymer material adds after the inorganic powder of non-modified, often causes the mechanical property of material and processing characteristics to decline.Therefore must carry out surface modification to inorganic powder, make it become the lipophilicity after modification from original hydrophilic surface properties, to improve machinery and the processing characteristics of packing material.
The surface modifying method of common inorganic powder has:
1, use tensio-active agent and coupling agent to carry out surface treatment to inorganic powder.The problems such as small molecules treatment agent in use exists and separates out, migration.
2, use maleic anhydride, vinylformic acid, acrylate, methyl propenoic acid glycidyl alcohol ester graftomer etc. to prepare macromole properties-correcting agent, for polymer-modified/inorganic powder filled system.But the percentage of grafting of this class graftomer is lower, be only generally 0.4% ~ 2%, therefore to reach processing intent, the graftomer large usage quantities such as the maleic anhydride needing.
3, by means of producing the Special Equipments such as irradiation, plasma, ultrasonic wave, or first by means of the compound that can introduce in inorganic filler surface initiating group, then on inorganic powder surface, trigger monomer carries out polymerization, forms polymer graft " shell-core " structure at inorganic powder surface.Concrete disclosed achievement has: Wang Yong " SCI " (1994,15 (8): 1253-1255) has delivered " interfacial interaction of the simultaneously toughness reinforcing enhancing of mineral filler HDPE system ".This research is to CaCO
3carry out radiation treatment, by CaCO
3free radical that surface produces is acrylamide triggered carries out polymerization, at CaCO
3polyacrylamide on surface grafting, thus reach the object of modification.Similarly report also has: the people such as Wang Huaifa have delivered " radiation modification of inorganic particulate material " in " Chinese powder technology " (2000, (6): 235-238); High skellats etc. have been delivered " the dispersing morphology research of irradiation grafting modified nano calcium carbonate in polyoxymethylene " in " insulating material " (2003, (3): 13-15); Wu Chunlei has delivered " nanometer SiO in " matrix material journal " (2002,19 (6): 61-67)
2the mechanical property of surface grafting polymerization and behavior of polypropylene composites thereof "; Jiang Bo has delivered " mgo surface radiation graft polymerization study on mechanism " in " applied chemistry " (1997,14 (1): 95-97); Wen Guian, the tribute of chapter literary composition have been delivered " surface modification of low temperature plasma of inorganic powder " in " powder technology " (1997,3 (2): 27-32); The people such as Fan Shimin have delivered " plasma surface modification of calcium carbonate " in " Chinese powder technology " (2002,31 (2): 5-8); The people such as Lu Shouci have delivered " theory and practice of mineral color stuffing mechanical-chemical modification " in " Chinese powder technology " (1999,5 (1): 33-37); The people such as Yang Huaming have delivered " progress of Ultra-fine Crushing Machinery chemistry " in " Chinese powder technology " (2002,8 (2): 31-36); Xu's happy has been delivered " polymer material science research trend and forecast of development " in " new material industry " (2003, (3): 12-17); Money man is contained in " Anhui chemical industry " (2000, (6): 13-14) and has delivered " nanometer SiO
2the research of surface aggregate thing graft modification "; Not big delivered in " Beijing University of Chemical Technology's journal (natural science edition) " (2003,30 (2): 1-4) " polymer graft modification superfine silicon dioxide surface appearance and formation mechanism ".
4, polymer is fixed on to inorganic filler surface by certain mode.Concrete disclosed achievement has: patent one has the method (ZL 200710144038.6) of the inorganic powder of " core-shell " structure through surface modification preparation.The raw fine jade has been delivered " macromole bonding is processed the surface properties of aluminium hydroxide and the interfacial characteristics with common polymer thereof " in " Chinese Plastics " (1999,13 (1): 80-84).Zhu Deqin has delivered " Surface Chemistry In-situ Multi-modified Al (OH) in " Chinese Plastics " (2006,20 (9): 23-27)
3the preparation of/PVC matrix material and performance ".Tang Longxiang has delivered " research of the synthetic TPU Toughened PP of talcum powder surface in situ " in " Chinese Plastics " (2000,14 (11): 71-75).
3, there is modified technique complexity in 4 liang of class methods, the shortcoming of more difficult industrialization promotion.Therefore, be more common in academic research, and rare practical application.
Because inorganic powder has a wide range of applications at Macromolecular materials industry, develop simple, hygienic safety, lasting Surface Modification of Inorganic Powder technology is reliably the pursuit of industry and scientific and technological circle always.
Ethylene-vinyl alcohol copolymer (EVOH) is that a kind of processibility that ethene is good and high barrier properties for gases of polyvinyl alcohol of gathering is in the crystalline polymer of one, with polyvinylidene dichloride (PVDC) and polyamide (PA) and be called three large barrier resins, its gas barrier property is than more than the at present conventional high decades of times of high barrier material PVDC, higher 100 times than PA, higher 10000 times than PE, PP.Therefore, ethylene-vinyl alcohol copolymer is mainly used in packaging field and prepares automotive oil tank at present.After the structure of our research and analysis ethylene-vinyl alcohol copolymer (EVOH), find: in EVOH up to the vinyl alcohol structural unit of 30-70 % mole fraction, can with the Chemical bond water generates hydrogen bond action of inorganic powder surface, also can produce electrostatic interaction with the polar group of inorganic powder, make natively itself and inorganic powder have good consistency; And ethene structural unit and the most matrix polymer up to 30-70% molar content has good affinity in EVOH, can produce the two macromolecular chain and be wound around.Therefore ethylene-vinyl alcohol copolymer can be used as a kind of inorganic powder surface agent, for improving the consistency between inorganic powder and polymeric matrix, gives the mechanical property that polymer-filled compound system is good.
Retrieve a large amount of patent documentations and the correlative study paper of publishing, this EVOH be there is no to pertinent literature and patent report at present for the method for modifying of inorganic powder.Only find that the people such as Zhang Yujun are at " Heilongjiang University's natural science journal " upper (2006,23 (1): 124-127) delivered " preparation of EVOH/montmorillonite laminated compound material and structural characterization ", this research is take polyvinyl pyrrolidone modified polynite (MMT) as inorganic phase, take ethene-vinyl alcohol copolymer as matrix resin, prepare EVOH/montmorillonite composite material by fusion intercalation, reduce the water absorbability of matrix material, and improve cost performance.The people such as Tang Zhongzhu are at " Journal of Functional Polymers " (2005,18 (3): 368-372) on, delivered " preparation of TPS/EVOH Composites and performance ", this research is prepared starch-base biodegradation material with ethylene-vinyl alcohol copolymer and thermoplastic starch blend, the degradation property of controlling compound system by the proportioning of ethylene-vinyl alcohol copolymer and thermoplastic starch in control compound system, the add-on of ethylene-vinyl alcohol copolymer is between 10-40%.Similarly research also has " the preparation and property research of TPS/ EVOH blend " that the people such as Zhang Meijie deliver in " plastics industry " (2003,31 (1): 27-29).In above-mentioned literary composition, be all using ethylene-vinyl alcohol copolymer as with the blended material of thermoplastic starch to improve the degradation property of starch/ethylene-vinyl alcohol copolymer matrix material, and do not explicitly point out the surface-modifying agent using ethylene-vinyl alcohol copolymer as thermoplastic starch.Retrieve 1 piece of granted patent about ethylene-vinyl alcohol copolymer based composites (ZL 201110189511.9) simultaneously, this patent provides one to utilize calcium sulfate and W-Gum to manufacture ethylene-vinyl alcohol copolymer based composites and preparation technology thereof, its objective is the cost in order to reduce ethylene-vinyl alcohol copolymer based composites, and give matrix material certain degradation property.This patent is by adding stearic acid to carry out surface active modification to calcium sulfate, to improve the consistency of calcium sulfate, W-Gum and ethylene-vinyl alcohol copolymer, improve the mobility of melt and the surface flatness of matrix material, this patentee does not recognize the compatible role of ethylene-vinyl alcohol copolymer to calcium sulfate and W-Gum existence as seen simultaneously.The present invention directly utilizes ethylene-vinyl alcohol copolymer as improving dispersiveness and the consistency of inorganic powder at polymeric matrix, and this modification theory and method of modifying are that the applicant proposes first.
Summary of the invention
The present invention is directed to the deficiency of existing inorganic powder treatment process, provide a kind of take ethylene-vinyl alcohol copolymer as properties-correcting agent, adopt dry process inorganic powder to be carried out to the method for surface modification, to improve the consistency between inorganic powder and organic polymer material, improve its dispersiveness.
For achieving the above object, the present invention adopts following technical scheme:
Composition of raw materials is by weight: 100 parts of inorganic powders, ethylene-vinyl alcohol copolymer 1-6 part, glycerine 5-30 part.
The ethene molar content of described ethylene-vinyl alcohol copolymer is 30-70%.
Described inorganic powder is calcium carbonate, calcium oxide, calcium hydroxide, aluminium hydroxide, aluminum oxide, magnesium hydroxide, magnesiumcarbonate, magnesium oxide, brucite, rhombspar, calcite, slag magnesiumcarbonate, Sodium Aluminium Carbonate Basic, wollastonite, kaolin, clay, mica, talcum powder, silicon-dioxide, titanium dioxide, glass microballon, marble, chalk, Wingdale, barium sulfate, nepheline, potassium felspar sand, albite, graphite, carbon black, one or more in ultrafine inorganic powder or the nano inorganic powder of zinc oxide or zinc carbonate.
The surface modifying method of described inorganic powder comprises the following steps:
(1) ethylene-vinyl alcohol copolymer is ground into 20-100 order powder, 90-92 ℃ of dry 8 h, for subsequent use;
(2) inorganic powder is in 90-120 ℃ of dry 1-3 h;
(3) after dried ethylene-vinyl alcohol copolymer powder is mixed with glycerine, dried inorganic powder is carried out to activation treatment 10-30 min at 165-200 ℃, obtain the inorganic powder of surface modification.
Beneficial effect of the present invention is: the vinyl alcohol structural unit in (1) ethylene-vinyl alcohol copolymer and ethene structural unit can produce good interface combination respectively at inorganic powder and polymeric matrix, without separately adding interfacial compatibilizer.If this technology obtains large-scale promotion application, the alternative method of modifying generally using at present, thus alleviate the environmental pollution bringing because producing conventional compatilizer.Because commercialization ethylene-vinyl alcohol copolymer is to be produced by the modernization large chemical complex with strict environmental practice, this is compared with producing maleic anhydride class graftomer process in general plastic working factory, and environmental pollution is little and be convenient to concentrate and administer.(2) ethylene-vinyl alcohol copolymer is of a great variety, vinyl alcohol molar content 30-70 %, and properties-correcting agent choice is large.In ethylene-vinyl alcohol copolymer molecular structure, the ratio of ethene and two kinds of structural units of vinyl alcohol is adjustable, and this provides choice widely for preparation of a great variety and polymer base inorganic powder composite material that loading level is totally different.(3) can directly process inorganic powder, easy to operate, technique is simple, and production efficiency is high, and production of articles cost is low.(4) ethylene-vinyl alcohol copolymer itself is nontoxic, products obtained therefrom environmentally safe.Ethylene-vinyl alcohol copolymer is macromole properties-correcting agent, in goods use procedure, do not exist separate out, pollution and the Problem of Failure such as migration.
Embodiment
embodiment 1
Formula: 5 parts of 100 parts of inorganic powders, ethylene-vinyl alcohol copolymer 1 part (ethene molar content is 70%), glycerine.Described inorganic powder is nano-calcium carbonate.
The surface modifying method of inorganic powder comprises the following steps:
(1) ethylene-vinyl alcohol copolymer is ground into 20 order powders, 90 ℃ of dry 8 h, for subsequent use;
(2) inorganic powder is in 90 ℃ of dry 1h;
(3) after dried ethylene-vinyl alcohol copolymer powder is mixed with glycerine, dried inorganic powder is carried out to activation treatment 10 min at 165 ℃, obtain the inorganic powder of surface modification.
embodiment 2
Formula: 30 parts of 100 parts of inorganic powders, ethylene-vinyl alcohol copolymer 6 parts (ethene molar content is 30%), glycerine.Described inorganic powder is the ultrafine inorganic powder mixture (mass ratio is 1:1:1:1) of marble, potassium felspar sand, albite and carbon black.
The surface modifying method of inorganic powder comprises the following steps:
(1) ethylene-vinyl alcohol copolymer is ground into 100 order powders, 92 ℃ of dry 8 h, for subsequent use;
(2) inorganic powder is in 120 ℃ of dry 3 h;
(3) after dried ethylene-vinyl alcohol copolymer powder is mixed with glycerine, dried inorganic powder is carried out to activation treatment 30 min at 200 ℃, obtain the inorganic powder of surface modification.
embodiment 3
Formula: 15 parts of 100 parts of inorganic powders, ethylene-vinyl alcohol copolymer 3 parts (ethene molar content is 44%), glycerine.
Described inorganic powder is the ultrafine inorganic powder (mass ratio is 1:1:1:1:1) of calcium oxide, calcium hydroxide, kaolin, talcum powder and glass microballon.
The surface modifying method of inorganic powder comprises the following steps:
(1) ethylene-vinyl alcohol copolymer is ground into 60 order powders, 91 ℃ of dry 8 h, for subsequent use;
(2) inorganic powder is in 105 ℃ of dry 2 h;
(3) after dried ethylene-vinyl alcohol copolymer powder is mixed with glycerine, dried inorganic powder is carried out to activation treatment 20min at 175 ℃, obtain the inorganic powder of surface modification.
With the inventive method inorganic powder after treatment and polyacrylic interfacial tension (mJ/m
2) as follows:
Inorganic powder after 40 parts of modifications is joined in the polypropylene of 100 parts for the production of composite sheet, uses mechanics and the processing characteristics of universal testing machine test gained matrix material as follows:
Above result shows that present method can reduce the polarity of inorganic powder effectively, improves and the consistency of polymeric matrix, improves mechanical property and the processing characteristics of matrix material.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (4)
1. a surface modifying method for inorganic powder, is characterized in that: formula is made up of the raw material of following parts by weight: 100 parts of inorganic powders, ethylene-vinyl alcohol copolymer 1-6 part, glycerine 5-30 part.
2. the surface modifying method of inorganic powder according to claim 1, is characterized in that: the ethene molar content of described ethylene-vinyl alcohol copolymer is 30-70%.
3. the surface modifying method of inorganic powder according to claim 1, it is characterized in that: described inorganic powder is calcium carbonate, calcium oxide, calcium hydroxide, aluminium hydroxide, aluminum oxide, magnesium hydroxide, magnesiumcarbonate, magnesium oxide, brucite, rhombspar, calcite, slag magnesiumcarbonate, Sodium Aluminium Carbonate Basic, wollastonite, kaolin, clay, mica, talcum powder, silicon-dioxide, titanium dioxide, glass microballon, marble, chalk, Wingdale, barium sulfate, nepheline, potassium felspar sand, albite, graphite, carbon black, one or more in ultrafine inorganic powder or the nano inorganic powder of zinc oxide or zinc carbonate.
4. the surface modifying method of inorganic powder according to claim 1, is characterized in that: comprise the following steps:
(1) ethylene-vinyl alcohol copolymer is ground into 20-100 order powder, 90-92 ℃ of dry 8 h, for subsequent use;
(2) inorganic powder is in 90-120 ℃ of dry 1-3 h;
(3) after dried ethylene-vinyl alcohol copolymer powder is mixed with glycerine, dried inorganic powder is carried out to activation treatment 10-30 min at 165-200 ℃, obtain the inorganic powder of surface modification.
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Cited By (8)
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| CN104087025A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | Modified calcium carbonate with enhanced wear resistance and preparing method thereof |
| CN106006712A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparing method for nanometer zinc oxide |
| CN106116394A (en) * | 2016-07-06 | 2016-11-16 | 浙江新业管桩有限公司 | A kind of modified quicklime |
| CN106280563A (en) * | 2016-08-05 | 2017-01-04 | 中玺新材料（安徽）有限公司 | A kind of protection type composite calcium carbonate and preparation method thereof |
| CN113549347A (en) * | 2021-07-06 | 2021-10-26 | 安徽黑钰颜料新材料有限公司 | Surface modification method of carbon black |
| CN114752232A (en) * | 2022-04-21 | 2022-07-15 | 郑州圣莱特空心微珠新材料有限公司 | Elastomer-coated hollow glass bead and preparation method and application thereof |
| CN115028916A (en) * | 2022-06-08 | 2022-09-09 | 广州丽盈塑料有限公司 | High-barrier light plastic for plastic packaging container and preparation method thereof |
| CN116004035A (en) * | 2022-12-20 | 2023-04-25 | 烟台大学 | Inorganic calcium carbonate surface modification method and application thereof |
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| CN106006712A (en) * | 2016-07-07 | 2016-10-12 | 安徽省含山县锦华氧化锌厂 | Preparing method for nanometer zinc oxide |
| CN106280563A (en) * | 2016-08-05 | 2017-01-04 | 中玺新材料（安徽）有限公司 | A kind of protection type composite calcium carbonate and preparation method thereof |
| CN113549347A (en) * | 2021-07-06 | 2021-10-26 | 安徽黑钰颜料新材料有限公司 | Surface modification method of carbon black |
| CN114752232A (en) * | 2022-04-21 | 2022-07-15 | 郑州圣莱特空心微珠新材料有限公司 | Elastomer-coated hollow glass bead and preparation method and application thereof |
| CN114752232B (en) * | 2022-04-21 | 2024-02-02 | 郑州圣莱特空心微珠新材料有限公司 | Elastomer-coated hollow glass bead and preparation method and application thereof |
| CN115028916A (en) * | 2022-06-08 | 2022-09-09 | 广州丽盈塑料有限公司 | High-barrier light plastic for plastic packaging container and preparation method thereof |
| CN116004035A (en) * | 2022-12-20 | 2023-04-25 | 烟台大学 | Inorganic calcium carbonate surface modification method and application thereof |
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