CN103031015B - A kind of polyamide wax modification sericite powder, Its Preparation Method And Use - Google Patents
A kind of polyamide wax modification sericite powder, Its Preparation Method And Use Download PDFInfo
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- CN103031015B CN103031015B CN201210585857.5A CN201210585857A CN103031015B CN 103031015 B CN103031015 B CN 103031015B CN 201210585857 A CN201210585857 A CN 201210585857A CN 103031015 B CN103031015 B CN 103031015B
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Abstract
The invention discloses a kind of polyamide wax modification sericite powder, Its Preparation Method And Use, wherein polyamide wax modification sericite powder is the polyamide wax modification sericite powder obtained after carrying out surface modification as properties-correcting agent to sericite by polyamide wax, and wherein the mass ratio of polyamide wax and sericite is 0.1-10:100; Polyamide wax modification sericite powder of the present invention can be used as Rhelogy Control Agent and uses, and enhances the solvent resistant grade of auxiliary rheological agents, avoids the rear thickening behavior of storage period.
Description
One, technical field
The present invention relates to a kind of sericite functional stuffing preparation method and its usage of polyamide wax surface modification, be mainly used in chlorinated rubber coating, high solid coating, epoxy coating, the dry factory coatings of gas, road marking paint, hammer paint, decoration paints, polyurethane paint, pitch compound, antifouling paint, filler, mastic coatings, tackiness agent, the fields such as sealing material, as functional material, except strengthening acid and alkali-resistance, antiultraviolet, thermotolerance, wear resistance, insulativity, outside the performances such as physical strength, also can give institute's packing material thixotroping structure, improve pigment suspension performance, control sagging and do not sacrifice flowing and levelling property, and give package stability and reproducibility.
Two, background technology
1, the rheological property of coating
Rheological property can give the rock steady structure of coating system uniqueness, can protect the granules of pigments disperseed, and is formed and has thixotropic mastic coatings, contributes to controlling sagging, keeps excellent levelling property, prevent pigment sedimentation.Concerning coatings industry, rheological property is present in from material choice, coating, storage of finished products until each stage of application and construction and conversion film forming, is an important factor that must consider.
Coating sagging and levelling are two conflicting phenomenons.Good film levelling property requires, within the sufficiently long time, viscosity is remained on lower-most point, and when having sufficient, the abundant levelling of chien shih film, forms smooth film, and flowing down problems appears in such tend; Otherwise require not occur sagging completely, dope viscosity must be high especially, and it will cause seldom or completely not having mobility.The production of coating and storage are also like this, and in coating, the density of pigment, filler is higher, require viscosity to be remained on vertex, to obtain good dispersion effect during production; May be attached together between particle and particle when storing and form larger particle, and occur rapid sedimentation, even sink to the bottom caking and layering occurs, higher viscosity must be kept.Therefore the viscosity characteristics of coating is: when shearing rate increases, viscosity progressively declines; Once release shearing force, viscosity is gone up again.Because primary formation goes to pot, have to pass through the regular hour, just can return to original value.The region area surrounded when viscosity profile middle shear rate increases and return and fall is the yardstick weighing its thixotropic property.
In coating system, add a coatings additive(s) having a good thixotropic effect, set up a thixotroping structure, just can form a valuable performance, have comparatively low viscosity under the high shear rate namely when construction, contribute to paint-flow and constructability; Under low shear rate before and after construction, there is viscosity higher, pigment sedimentation and wet film sagging can be prevented.
2, auxiliary rheological agents and development trend
Generally adopt auxiliary rheological agents (or claiming rheological agent) to form gel network at present, give coating system rheological property.Auxiliary rheological agents is used to have following effect:
1), sagging when preventing application, levelling coating thickness;
2), pigment sedimentation when preventing storage, or make precipitation softening to improve redispersibility;
3), brushing property is improved;
4), prevent coating from infiltrating porous substrate, improve brush mark and levelling property.
Conventional auxiliary rheological agents divides two classes.One class is nano inorganic powder, and principal item has aerosil and organobentonite.Mineral-type auxiliary rheological agents forms reproducible network structure by the oxygen key on its surface and hydroxyl bonding, and hydrogen bond is destroyed under shearing force, viscosity degradation, and shearing force forms hydrogen bond structure, viscosity recovery after eliminating again.Because bonding action is comparatively strong, general result of prevention is better, but due to limitation of size, be difficult to form network structure fine and closely woven on microcosmic, often thixotropic property is poor, and thixotropy is all subject to the impact of temperature, when temperature raises, hydrogen bond action weakens, and viscosity reduces, and sag resistance is deteriorated.
Another kind of is organic auxiliary rheological agents, containing more than 3 polar groups and the organism of three-dimensional distribution.Organic auxiliary rheological agents has thixotropy by being mutually wound reticulated structure of macromolecular chain, polar group is reticulated structure interface, be opened by the molecule be wound around when shearing, thus viscosity reduce, when shearing stops macromole being wound around again and induced viscosity rising.Because this process be again wound around is relatively slow, there is the long period to give wet film flowing and levelling, but sagging can not be caused out of control, thus there is good rheological property.But the two dispersion is more difficult, needs stronger dispersion condition, as sand milling and the grinding of three rollers, also have the slurry product being prefabricated into about 20%, need not grind can after add, but use cost is doubled and redoubled.Simultaneously storage period because solvation also there will be false thick phenomenon, cause rheological property to decline.
The main application kind of organic rheological agent has polyamide wax and modified castor oil derivative.
Modified castor oil derivative is a kind of waxy solid obtained by Viscotrol C Hydrogenation, owing to having hydroxyl on fatty acid chain, therefore polarity is to a certain degree shown, can swell gel in non-polar solvent, produce faint hydrogen bonded because of the polar group in hydrogenated castor oil molecule between swollen particles, be formed with thixotropic network structure.Carry out modification with acid amides to hydrogenated castor oil, after amide modifications, hydrogenated castor oil successfully enhances the solvent resistant grade of industrial coating.For many years, this kind of rheological agent is successfully applied to various industrial coating, especially heavy-duty coating and Marine Paints, but this kind of rheological agent is very sensitive to temperature, almost destroy totally higher than its thixotropic effects when 60 DEG C in temperature, and still have the shortcomings such as false thick in use.
Polyamide wax is by fatty acid amide emulsification polarization in native paraffin mostly, put into dimethylbenzene swelling in advance again and generate paste thixotropic agent, its swelling structure reticulates, there are extraordinary intensity and thermotolerance, excellent storage stability, be applied in polychromatic finish and can also control tinsel good orientation and improve impact property, less to the susceptibility of temperature, produce under the condition of room temperature to 80 DEG C and at hot setting time also can not obviously destroy its thixotropy, therefore be also suitable for preparing all kinds of baking finish, especially high-solid level baking finish, it is the rheology modifier simultaneously possessing good sag prevention effect and levelling effect.The rheological of high solid coating is difficult to control, because in solvent evaporation process, viscosity increases the alkyd that relative molecular mass is low (still having a small amount of solvent in coating) hardly, but rheological agent can not make again the viscosity increase of coating too large, otherwise the too large application difficulty of viscosity, it is high and can anti-sag effectively that polyamide wax flowing deformation rheological agent just can not meet these requirements, particularly viscosity under very little addition.
All the time, the development & production of polyamide wax is controlled by overseas enterprise always, as this P200X anti-settling agent of extra large name, and the Disparlon6900-20X etc. of this production of Japanese nanmu.But along with the development need of coating cause, domestic enterprise more and more recognizes the importance of rheological thickeners, organobentonite, silicon-dioxide cannot adapt to the demand of growing coatings industry for rheological agent, increasing company starts research and development and adopts polyamide wax flowing deformation rheological agent, and reaches world level.Modern age, auxiliary rheological agents development trend presented following characteristics:
1), coatings industry has widely used mastic coatings, usually constructed with Airless spraying.Under the high shear rate of Airless spraying equipment, require that dope viscosity is lower, constructability, but have certain viscosity during film forming to prevent sagging in vertical surface, the superior polyamide wax flowing deformation rheological agent of rheological property becomes mainly applies kind.
2) increasing substantially, along with polychromatic finish market consumption, has polar organic group, and the polyamide wax flowing deformation rheological agent that can control tinsel good orientation becomes mainly applies kind.
3), can avoid the new rheology auxiliary agent of two class auxiliary rheological agents shortcomings, both have good rheological property, working conditions is wide in range simultaneously, and cost performance is high, and result of use is stablized.
3, sericite and Application Areas thereof
Sericite (Sericite) is the one of mica, and belong to the subspecies of white mica, its chemical structure is KAl
2(AlSi
2o
10) (OH)
2, crystal is flakey, and crystalline aggregate is in block, and aobvious grey, purple rugose rose look, white etc., tool satin luster is the silicate minerals with laminate structure.Sericite ultraviolet radiation specific absorption reaches more than 90%, thermal stability 500 ~ 600 DEG C, electrical insulating property 200kv/mm, Young's modulus is 1505 ~ 2134MPa, be insoluble in acid-base solution, stable chemical nature, the performances such as institute's packing material antiultraviolet, acid and alkali-resistance, thermotolerance, insulativity, physical strength can be given, mainly use as the functional stuffing of the Application Areass such as coating at first, especially in anticorrosion and outdoor application scenario, there is sheet structure and intercept anti-corrosion function and shielding ultraviolet rays is ageing-resistant, weather resistance, become the optimal selection of paint filler.{ 001} cleavage is complete, can be split into very thin sheet, thick below the 1u of reaching of sheet (can be whittled into 0.001u in theory) for sericite.Radius-thickness ratio is large, and especially wet method product can reach about 100, and its structure and composition have clay characteristic concurrently, and therefore suspension is good, has good thixotropic property, has adapted to the requirement of the anti-settling and rheological property of Coating Market, has more and more become the general raw material of coating system at present.
Three, summary of the invention
The present invention aims to provide a kind of polyamide wax modification sericite powder, Its Preparation Method And Use, take sericite as substrate, polyamide wax is adopted to carry out surface modification, develop a kind of high thixotropic sericite material, except can giving the performances such as institute's packing material antiultraviolet, acid and alkali-resistance, thermotolerance, insulativity, physical strength, also can give institute's packing material thixotroping structure, improve pigment suspension performance, control sagging and do not sacrifice flowing and levelling property, and giving package stability and reproducibility.
Polyamide wax modification sericite powder of the present invention, lower abbreviation modification sericite powder, it is the polyamide wax modification sericite powder obtained after surface modification being carried out to sericite by polyamide wax as properties-correcting agent, wherein the mass ratio of polyamide wax and sericite is 0.1-10:100, hereinafter referred to as the addition of properties-correcting agent, namely refer to that the addition of properties-correcting agent accounts for the per-cent of quality of sericite.The preparation method of polyamide wax modification sericite powder of the present invention is as follows:
200-10000 object sericite powder is dried to constant weight in 100-120 DEG C, whole adsorption moisture in removing material, drying time should be determined, generally at 3 hours according to the dry wet situation of material; The ratio of dried sericite powder and the cured powder of properties-correcting agent polymeric amide 100:0.1-10 is in mass ratio added in heated at high speed mixing machine (or claiming heated at high speed kneading machine) reactor, be uniformly mixed 3-90min in 110-180 DEG C, obtain the cured modification sericite powder of polymeric amide.
The concrete preparation process of the present invention is as follows:
1), material drying: 200-10000 object sericite powder dried under 100-120 DEG C of constant temperature in heating unit, whole adsorption moisture in removing material, drying time should be determined, generally at 3 hours according to the dry wet situation of material;
2), take material: take dried sericite powder, load in modified device heated at high speed mixing machine mixing kettle;
3), take properties-correcting agent: sericite powder in mass ratio: the ratio of organic wax powder=100:0.1-10, take the cured powder of a certain amount of properties-correcting agent polymeric amide;
4), high-speed mixing material: cured for properties-correcting agent polymeric amide powder is added in the sericite powder material in mixing kettle.Set surperficial modification temperature, open heated at high speed mixing machine, make powder material high-speed mixing (strong stirring) under 110-180 DEG C of condition, make properties-correcting agent and powder Homogeneous phase mixing, namely obtain the cured modification sericite powder of polymeric amide.Wherein high-speed stirring is that the equipment rotating speed of different model may be different relative to the speed range of equipment itself.
The purposes of polyamide wax modification sericite powder of the present invention is the application that it can be used as Rhelogy Control Agent.
The properties-correcting agent polyamide wax that the present invention selects is the polycondensate of ten dihydroxyl stearic acids and hexanediamine.Ten dihydroxyl stearic acids are hydrogenated castor oil hydrolysate, carry oh group, not need in native paraffin emulsification polarization, constant product quality, with it for polyamide wax molecule prepared by raw material has 4 three-dimensional polar groups (2 hydroxyls, 2 amide group) distributed, the reticulated structure that intensity is higher can be formed, have modified castor oil derivative high-shear low viscosity and the full-bodied advantage of polyamide wax low sheraing concurrently.
The theoretical amount of properties-correcting agent can be obtained by following formulae discovery:
W＝(W
1×S
1)/S
2
In formula: W---rheological agent consumption (g);
W
1---sericite in powder body weight (g);
S
1---the specific surface area (m of sericite powder
2/ g);
S
2---the minimum coated area (m of rheological agent
2/ g).
The just theoretical amount obtained by above-mentioned formulae discovery.Usually, mineral granularity is thinner, and specific surface area is larger, and the consumption of required properties-correcting agent is larger.First the present invention goes out the theoretical amount of properties-correcting agent needed for different grain size sericite filler by the theoretical amount formulae discovery of properties-correcting agent, then observation and test analysis carry out verifying and revising by experiment, finally sift out optimum amount.
Compared with prior art, the modified effect of product of the present invention is excellent, and modified product quality is high, and technique is convenient, and its end-use is extensive, and can produce obvious economic and social profit, main beneficial effect is embodied in:
1, the consistency of sericite is enhanced
The sericite powder of long time without surface modification is a kind of polarity inorganics, has the surface characteristic of " hydrophilic oleophobic ", and poor with the affinity of organic resin matrix, direct filling easily causes the boundary defect of two phase material.By the sericite powder of polyamide wax modification, there is " oleophilic drainage " surface characteristic, good with the affinity of organic polymer matrix, dispersedly can be filled in machine superpolymer base-material, play the effect of function powder filler.
2, the use cost of rheological agent is reduced
Polyamide wax flowing deformation rheological agent product has two kinds of forms.One is superfine powder, needs to grind in advance to prepare pre-gelled before using, and not only technique is loaded down with trivial details, and production efficiency is extremely low; Another kind is the pre-gelled slurry of about 20%, although add conveniently, auxiliary agent price is doubled and redoubled.Modification sericite, through simple surface cladding tech, makes rheological agent be unit molecule fractions distribution substantially, and it is convenient to add, and cost performance is high.
3, the result of use of rheological agent is improved
Through surface coating modification, not only rheological agent obtains abundant dispersion, and by shear at high temperature, makes the polar group of polyamide wax flowing deformation rheological additive and sericite surface hydroxyl define the bonding action of chemical, enhance the solvent resistant grade of rheological agent, avoid the rear thickening behavior of storage period.
4, modified technique is convenient
Dry method modification technology of the present invention, technical process is simple, and mechanization degree is high, easy to operate, is suitable for large-scale mass production.
5, remarkable in economical benefits
The present invention obviously can improve the consistency of sericite filler, for application system provides rheological structure that is easy to use, with low cost, stable performance, widen the industrial application of sericite, and made it obviously rise in value, thus can produce obvious economic and social profit.
Four, embodiment
The lattice sharp board wet method sericite in powder that the sericite powder used in the embodiment of the present invention is the process for processing of institute of Chuzhou Grea Minerals Co., Ltd.; The cured powder of properties-correcting agent polymeric amide used in the embodiment of the present invention is the production of Changxing consonance macromolecular material company limited, and the trade mark is RC-100.
Embodiment 1:
In the present embodiment, modification sericite powder is prepared by the following method:
1000 object sericite powder are dried to constant weight in 110 DEG C, and time of drying is 3 hours; The ratio of dried sericite powder and the cured powder of properties-correcting agent polymeric amide 100:2 is in mass ratio added in heated at high speed mixing machine reactor, is uniformly mixed 10min in 135 DEG C, obtains modification sericite powder.
Embodiment 2:
In the present embodiment, modification sericite powder is prepared by the following method:
1250 orders are obtained sericite powder and is dried to constant weight in 110 DEG C, time of drying is 3 hours; The ratio of dried sericite powder and the cured powder of properties-correcting agent polymeric amide 100:3 is in mass ratio added in heated at high speed mixing machine reactor, is uniformly mixed 10min in 140 DEG C, obtains modification sericite powder.
Embodiment 3:
In the present embodiment, modification sericite powder is prepared by the following method:
2500 orders are obtained sericite powder and is dried to constant weight in 110 DEG C, time of drying is 3 hours; The ratio of dried sericite powder and the cured powder of properties-correcting agent polymeric amide 100:5 is in mass ratio added in heated at high speed mixing machine reactor, is uniformly mixed 10min in 145 DEG C, obtains modification sericite powder.
Embodiment 4:
In the present embodiment, modification sericite powder is prepared by the following method:
5000 orders are obtained sericite powder and is dried to constant weight in 110 DEG C, time of drying is 3 hours; The ratio of dried sericite powder and the cured powder of properties-correcting agent polymeric amide 100:10 is in mass ratio added in heated at high speed mixing machine reactor, is uniformly mixed 10min in 145 DEG C, obtains modification sericite powder.
Sericite powder is after polyamide wax surface modification, and its rheological property will be greatly improved.The present invention adopts the testing method such as thixotropic property mensuration, the classification of sag prevention exponential sum pigment sedimentation to do further test and repair to polyamide wax modification sericite powder surface modification effect of the present invention, and main testing method is as follows:
1, thixotropic property
The modification sericite powder (addition of properties-correcting agent is 0.3%) of each paint quality 3% is added respectively in hydroxyl acrylic varnish, lipid acid alkyd varnish, after being uniformly dispersed by identical technique, constant temperature 24h in 25 DEG C of environment, by the viscosity of NDJ-1 type rotational viscosimeter test sample under different rotating speeds, observe the change of sample viscosity under high, medium and low shearing force thus, measure the thixotropic property of modification sericite in several coating system, result is as shown in table 1.As can be seen from Table 1, no matter in any coating, the rheological property of modification sericite powder all with directly use polyamide wax suitable, or be slightly better than polyamide wax.Compared with other rheological agents, the thickening effectiveness of the two is all best, and aerosil and bentonite used in amounts increase several times just can reach similar thickening effectiveness.When same amount, the thixotropy of the two is also best, and organobentonite and aerosil will just have good thixotropic property when large usage quantity.That is, modification sericite not only has good anti-sag effect and helps flowing, flow leveling, and has excellent thickening, anti-settling effect, effectively can prevent the precipitation of face in coating, filler.
2, sag resistance
The modification sericite powder (addition of properties-correcting agent is 0.3%) of each paint quality 3% is added respectively in hydroxyl acrylic varnish and lipid acid alkyd sub-gloss varnish, at high-solid epoxy resin amine baking varnish, (solids content is 70%, its epoxy resin 28.3%, aminoresin 11.5%, catalyzer 0.2%, titanium dioxide 30%, solvent 30%) in add the modification sericite powder (addition of properties-correcting agent is 0.5%) of baking finish quality 5%, after being uniformly dispersed by identical technique, use sagging tester blade coating respectively on tinplate, by GB/T9264 standard test sagging performance, wherein hydroxyl acrylic varnish and lipid acid alkyd sub-gloss varnish are at room temperature crosslinking curing, epoxy amino baking finish is respectively at 150 DEG C and 200 DEG C of baking-curing 30min, result is as shown in table 2.As can be seen from Table 2, no matter in any coating, the anti-sag performance of modification sericite powder all with directly use polyamide wax suitable, or be slightly better than polyamide wax.Compared with other rheological agents, in hydroxyl acrylic varnish and lipid acid alkyd sub-gloss varnish, modification sericite powder and polyamide wax anti-sag effect best, next is the sample adding aerosil, add bentonite sample and also have certain anti-sag effect, its anti-sag effect of sample not adding rheology modifier is poor.In the epoxy amino baking finish of high-solid level, add modification sericite powder and polyamide wax, there is excellent anti-sag performance under 150 DEG C of high temperature curing conditions, when higher temperature is as 200 DEG C of solidifications, still there is good anti-sag effect.By contrast, the aerosil of same consumption and bentonite sag resistance poor; Only have and aerosil and bentonite addition are increased several times, higher anti-sag performance could be obtained; And do not add its anti-sag poor effect of sample of rheology modifier.
3, levelling property
The modification sericite powder (addition of properties-correcting agent is 0.5%) of each paint quality 5% is added respectively in hydroxyl acrylic varnish, lipid acid alkyd sub-gloss varnish, by GB/T1750 standard and GB/T3998 standard test modification sericite on the impact of film levelling property, result is as shown in table 2.As can be seen from Table 3, in above-mentioned two kinds of coating systems, add modification sericite powder, its film flow leveling with directly to use polyamide wax quite, substantially there is no detrimentally affect.Therefore, from another angle, this experiment confirms that modification sericite powder has good thixotropic property, while brute force improves coating sag resistance, and the levelling property of not obvious reduction coating.
Table 1 rheological property
Note: 1, TI value represents thixotropy index, and be the viscosity of 6r/min and the ratio of 60r/min viscosity, the larger rheological of TI value is stronger.
2, polyamide wax: Changxing consonance macromolecular material company limited RC-100; Aerosil: goldschmidt chemical corporation R972; Organobentonite: Zhejiang Ward chemical company BP-186.
3, above-mentioned rheology modifier is as a comparison all add after the pulpous state of previously prepared one-tenth 10% again, and addition refers to the per-cent counting each paint quality by 100% content.
Table 2 sag resistance
Table 3 levelling property
Note: 1, A represents, B represents better
2,10 grades represent that levelling property is best, and 0 grade represents that levelling property is the poorest.
Claims (1)
1. the preparation method of a polyamide wax modification sericite powder, it is characterized in that: be the polyamide wax modification sericite powder obtained after carrying out surface modification as properties-correcting agent to sericite by polyamide wax, wherein the mass ratio of polyamide wax and sericite is 0.1-10:100; Described polyamide wax modification sericite powder is that 200-10000 object sericite powder is dried to constant weight in 100-120 DEG C, the ratio of dried sericite powder and properties-correcting agent polyamide wax powder 100:0.1-10 is in mass ratio added in heated at high speed mixing machine reactor, 3-90min is uniformly mixed, the polyamide wax modification sericite powder obtained in 110-180 DEG C; Described polyamide wax is the polycondensate of ten dihydroxystearic acids and hexanediamine.
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| CN101328380A (en) * | 2008-07-24 | 2008-12-24 | 中国石油天然气集团公司 | Pipeline repaired mouth anti-corrosive primer coating having high adhesive bonding ability with thermal contraction belt |
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| CN101328380A (en) * | 2008-07-24 | 2008-12-24 | 中国石油天然气集团公司 | Pipeline repaired mouth anti-corrosive primer coating having high adhesive bonding ability with thermal contraction belt |
| CN101942263A (en) * | 2009-07-08 | 2011-01-12 | 中国石油天然气集团公司 | Wet and dry joint-coating primer for heat shrinkable tape and manufacturing method thereof |
| US20110154772A1 (en) * | 2009-12-31 | 2011-06-30 | Bostik, Inc. | Moisture Curable Adhesive Composition and Method for Installing Hardwood Floors |
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