CN106478987B - A kind of waste stone dust surface modifying method based on dry grinding - Google Patents
A kind of waste stone dust surface modifying method based on dry grinding Download PDFInfo
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- CN106478987B CN106478987B CN201610922816.9A CN201610922816A CN106478987B CN 106478987 B CN106478987 B CN 106478987B CN 201610922816 A CN201610922816 A CN 201610922816A CN 106478987 B CN106478987 B CN 106478987B
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- C08K9/00—Use of pretreated ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/34—Silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
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- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
Abstract
The present invention relates to a kind of waste stone dust surface modifying methods based on dry grinding, waste stone dust is added in first can be finely in the milling apparatus of temperature control, add in the ethanol solution of rare earth nitrades, 2~3h is ground under 30~50 DEG C of grinding temperature, then anionic fluorinated surfactant is added, 1h is ground under 30~50 DEG C of grinding temperature, finally collects the ultra-fine waste stone dust after grinding.The method of the present invention is by mechanical-chemical modification, rare-earth surface modification and the modification of fluorinated surfactant surface to combination, surface modification is carried out to waste stone dust jointly, ultra-fine waste stone dust high surface activity obtained, can be used as the filler of high molecular material, has widened the application field of waste stone dust.
Description
Technical field
The invention belongs to field of material surface modification, are related to a kind of waste stone dust surface modifying method, more particularly to a kind of base
In the waste stone dust surface modifying method of dry grinding.
Background technology
Waste stone dust is the waste generated in stone machining processing, and it is always a problem to recycle, and at present, waste stone dust is
Through having obtained some applications in fields such as concrete, mortar, artificial stones, but for the generation total amount of waste stone dust, still not
Whole waste stone dusts can be digested completely, cause the accumulation of a large amount of waste stone dusts, be a urgent need to resolve how to efficiently use waste stone dust
Environment and social concern.After waste stone dust is handled as applying filler in high molecular material, it can prepare polymer-based
Composite material has widened the application range of waste stone dust, advantageously accounts for its application problem.But waste stone dust belongs to inorganic particle,
Its compatibility with high-molecular organic material is poor, and surface binding force is weak, easily causes the decline of composite materials property, so
It needs to carry out it surface modification to improve its compatibility with macromolecule matrix material.
At present, the method for Surface Modification of Inorganic Powder mainly has surface covering modification, local chemical modification, mechanical force and chemical
Modification, outer layer membrane modifying, high-energy surface are modified and carry out surface modification etc., wherein mechanical-chemical modification using precipitation reaction
Refer to by crush, grind, rub the methods of enhance particle surface-active, make that there is strongly active powder surface and other objects
Matter is reacted, is adhered to, and achievees the purpose that surface is modified.The modification of mechanical force and chemical surface is modified ultra-fine grinding and surface and combines
Together, time saving, saving of labor saves energy consumption, easy to operate, has vast potential for future development.
Waste stone dust can be reached into crushing using the progress surface modification of mechanical-chemical modification method and surface modification is dual
Purpose, but single modification by mechanical force still cannot efficiently improve waste stone dust and the compatibility of high molecular material, can combine using other
Surface modifier plays synergistic effect, reaches the efficient surface modification to waste stone dust.Fluorinated surfactant is special surface activity
One kind of agent, modified effect is good, and the hydrogen moiety in the hydrocarbon chain of conventional surfactants or whole are replaced by fluorine atoms
Afterwards, the surfactant with carbon fluorine chain hydrophobic group is known as fluorinated surfactant, due to the presence of fluorine, fluorinated surfactant surface
It is active high, while there are the characteristics such as dispersion, wetting.Rare earth ion is also a kind of surface modifier simultaneously, with stronger network
Conjunction ability has stronger coordination to fluorine plasma, forms chemical bond, plays the effect of surface modification.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of waste stone dust surface modifying method, Yi Zhongji
In the waste stone dust surface modifying method of dry grinding, this method is simple for process, by mechanical-chemical modification, rare-earth surface modification and
The modification of fluorinated surfactant surface carries out surface modification, ultra-fine waste stone dust surface-active obtained to waste stone dust jointly to combination
Height can be used as the filler of high molecular material, widen the application field of waste stone dust.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of waste stone dust surface modifying method based on dry grinding, includes the following steps：
(1) adding in waste stone dust finely in the milling apparatus of temperature control, can add in the ethanol solution of rare earth nitrades, in 30~
2~3h is ground under 50 DEG C of grinding temperature；
(2) anionic fluorinated surfactant is added, 1h is ground under 30~50 DEG C of grinding temperature；
(3) the ultra-fine waste stone dust after grinding is collected.
The waste stone dust is waste marble powder, one or two kinds of mixtures of useless granite stone powder.
The rare earth nitrades are lanthanum nitrate, one kind of cerous nitrate.
The addition of the rare earth nitrades is the 0.5~2% of the waste stone dust weight.
The anionic fluorinated surfactant is sulfonate type fluorinated surfactant, sulfuric ester salt form fluorine surface-active
Agent, one kind of phosphate salt form fluorinated surfactant.
The addition of the anionic fluorinated surfactant is the 0.5~1% of the waste stone dust weight.
The particle size range of the ultra-fine waste stone dust is 1000~1200 mesh.
The present invention by mechanical-chemical modification, rare-earth surface modification and the modification of fluorinated surfactant surface to combination, jointly
Surface modification is carried out to waste stone dust, surface active is carried out to waste stone dust first with mechanical-chemical modification method, is reached simultaneously
The purpose of ultra-fine grinding, waste stone dust are improved by processing, surface-active, and surface hydroxyl increases, and hydroxyl can be with rare earth ion network
Conjunction forms chemical bond, then adds in anionic fluorinated surfactant, and the complexing power of rare earth ion and fluorine is strong, can establish compared with
Strong chemical bond thus forms a complex compound network on waste stone dust surface, can improve and especially contain with high molecular material
The binding force of fluoropolymer makes waste stone dust can be used as the filler of polymer-based composite.
Beneficial effects of the present invention：
(1) present invention is total to by mechanical-chemical modification, rare-earth surface modification and the modification of fluorinated surfactant surface to combination
Surface modification is carried out with to waste stone dust, modified effect is good, can be effectively improved the compatibility of waste stone dust and macromolecule matrix material, increases
Add the binding force of the two；
(2) present invention carries out surface modification using mechanical-chemical modification method to waste stone dust, can reach surface work simultaneously
Change the dual purpose with ultra-fine grinding；
(3) collective effect of rare earth ion and fluorinated surfactant can form a complex compound network on waste stone dust surface,
Itself and the especially fluoropolymer-containing binding force of high molecular material can be improved, waste stone dust is made to can be used as polymer-based composite
Filler；
(4) the method for the present invention is simple for process, synchronous to add in rare-earth modifier and fluorine table during dry grinding is carried out
Face activating agent is not required to increase processing step.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but does not limit protection scope of the present invention.
Embodiment 1
A kind of waste stone dust surface modifying method based on dry grinding, includes the following steps：
(1) adding in waste marble powder finely in the milling apparatus of temperature control, can add in the ethanol solution of lanthanum nitrate, lanthanum nitrate
Addition be waste stone dust weight 1%, grind 3h under 30 DEG C of grinding temperature；
(2) sulfonate type fluorinated surfactant is added, addition is the 0.5% of waste stone dust weight, in 30 DEG C grind
1h is ground at a temperature of mill；
(3) collect the ultra-fine waste marble powder after grinding, the particle size range of ultra-fine waste marble powder for 1000~
1200 mesh.
In order to verify the performance of the modified ultra-fine waste marble powder in surface prepared by embodiment 1, activation grade is carried out, has inhaled
The test of oil value and settling volume, activation grade can reflect the surface modification effect of waste marble powder, and activation grade is higher to be illustrated to be modified
Agent is bigger to the cladding degree of waste marble powder, and activation effect is better；Oil factor is with the dosage of dibutyl phthalate (DOP)
The quality of waste stone dust modified effect is reacted, oil factor then illustrates that greatly waste marble powder filled high polymer material can absorb more
The auxiliary agents such as plasticizer, cause processing cost to increase, generally, oil factor is the smaller the better；Settling volume can reflect waste marble powder
Dispersibility in a liquid, if waste marble powder good dispersion in atoleine, atoleine have powder preferable profit
Moist, powder is not easy to assemble and be bonded, and in sedimentation, particle arrangement accumulation is close, and settling volume is smaller.If conversely, dispersibility
Poor, then powder is easy to assemble, and there are compared with concrete dynamic modulus due to bridging between powder, when sedimentation easily forms loose deposit, settles
Volume is larger.Test method is as follows：
(1) activation grade：A certain amount of 1 ultra-fine waste stone dust of embodiment is added in suitable quantity of water, glass bar stirring 2min stands 1h
Afterwards, the floating material on upper strata is taken out, drying is weighed, and calculates activation grade according to the following formula：Activation grade=(floating material weight/gross mass) ×
100%,
(2) oil factor：It accurately weighs ultra-fine waste stone dust to be placed on glass plate, DOP is instilled to ultra-fine waste stone dust with buret,
It is stirred when being added dropwise with clean glass bar, when making the sample just all glue by glass bar, writes down O-phthalic
The dosage of dibutyl phthalate, calculates oil factor according to the following formula：Oil factor (mL/g)=DOP volumes/waste stone dust quality,
(3) settling volume：It measures 20mL atoleines to add in graduated cylinder with a scale, the ultra-fine waste stone dusts of 2g is added to
In 20mL atoleines, 3min is shaken with the speed of 100~120 times per minute, is stood for 24 hours, record solid volume is to settle
Volume.
Test result is shown：The activation grade of ultra-fine waste marble powder made from embodiment 1 is 98.1%, and oil factor is
0.065mL/g, settling volume 0.7mL；And the activation grade of waste marble powder being modified without 1 method of embodiment is 74.8%,
Oil factor is 0.170mL/g, settling volume 3.0mL；Data are analyzed it is found that ultra-fine waste marble powder made from embodiment 1
Activation grade significantly increases, and oil factor and settling volume decline significantly, illustrates that 1 method of embodiment changes the surface of waste marble powder
Property effect it is good, can improve dispersibility and compatibility of the waste marble powder in atoleine, further illustrate that embodiment 1 is given up Dali
Mountain flour can be applied in high molecular material, have good compatibility.
Embodiment 2
A kind of waste stone dust surface modifying method based on dry grinding, includes the following steps：
(1) adding in waste marble powder finely in the milling apparatus of temperature control, can add in the ethanol solution of lanthanum nitrate, lanthanum nitrate
Addition be waste stone dust weight 1%, grind 2h under 40 DEG C of grinding temperature；
(2) sulfuric ester salt form fluorinated surfactant is added, addition is the 1% of waste stone dust weight, in 40 DEG C grind
1h is ground at a temperature of mill；
(3) collect the ultra-fine waste marble powder after grinding, the particle size range of ultra-fine waste marble powder for 1000~
1200 mesh.
Test result is shown：The activation grade of ultra-fine waste marble powder made from embodiment 2 is 98.9%, and oil factor is
0.055mL/g, settling volume 0.4mL, modified effect are good.
Embodiment 3
A kind of waste stone dust surface modifying method based on dry grinding, includes the following steps：
(1) adding in useless granite stone powder finely in the milling apparatus of temperature control, can add in the ethanol solution of cerous nitrate, nitric acid
The addition of cerium is the 1% of waste stone dust weight, and 3h is ground under 30 DEG C of grinding temperature；
(2) phosphate salt form fluorinated surfactant is added, addition is the 0.5% of waste stone dust weight, in 30 DEG C
1h is ground under grinding temperature；
(3) the ultra-fine useless granite stone powder after grinding is collected, the particle size range of ultra-fine useless granite stone powder is 1000
~1200 mesh.
Test result is shown：The activation grade of ultra-fine useless granite stone powder made from embodiment 3 is 98.3%, and oil factor is
0.068mL/g, settling volume 0.6mL, modified effect are good.
Above-described embodiment is only one of presently preferred embodiments of the present invention, is not limited the scope of the invention with this, therefore：
The equivalence changes that all structures under this invention, shape, principle are done, should all be covered by within protection scope of the present invention.
Claims (6)
1. a kind of waste stone dust surface modifying method based on dry grinding, which is characterized in that include the following steps：(1) by barren rock
Powder adds in the ethanol solution that finely in the milling apparatus of temperature control, can add in rare earth nitrades, the rare earth nitrades be lanthanum nitrate,
One kind of cerous nitrate grinds 2~3h under 30~50 DEG C of grinding temperature；(2) anionic fluorinated surfactant is added, in
1h is ground under 30~50 DEG C of grinding temperature；(3) the ultra-fine waste stone dust after grinding is collected.
2. the waste stone dust surface modifying method according to claim 1 based on dry grinding, which is characterized in that the barren rock
Powder is waste marble powder, one or two kinds of mixtures of useless granite stone powder.
3. the waste stone dust surface modifying method according to claim 1 based on dry grinding, which is characterized in that the rare earth
The addition of nitrate is the 0.5~2% of the waste stone dust weight.
4. the waste stone dust surface modifying method according to claim 1 based on dry grinding, which is characterized in that it is described it is cloudy from
Subtype fluorinated surfactant is sulfonate type fluorinated surfactant, sulfuric ester salt form fluorinated surfactant, phosphate salt form fluorine table
One kind of face activating agent.
5. the waste stone dust surface modifying method according to claim 1 based on dry grinding, which is characterized in that it is described it is cloudy from
The addition of subtype fluorinated surfactant is the 0.5~1% of the waste stone dust weight.
6. the waste stone dust surface modifying method according to claim 1 based on dry grinding, which is characterized in that described ultra-fine
The particle size range of waste stone dust is 1000~1200 mesh.
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|---|---|---|---|---|
| CN103788410A (en) * | 2014-01-04 | 2014-05-14 | 安徽雪城超细碳酸钙有限公司 | Rare earth compound/titanate coupling agent modified ultrafine calcium carbonate filler |
| CN104479415A (en) * | 2014-12-26 | 2015-04-01 | 天津滨浦生产力促进有限公司 | Calcium carbonate surface modifier |
| CN105504891A (en) * | 2015-12-06 | 2016-04-20 | 天津儒创新材料科技有限公司 | Preparation method of rare earth modifier |
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| CN103788410A (en) * | 2014-01-04 | 2014-05-14 | 安徽雪城超细碳酸钙有限公司 | Rare earth compound/titanate coupling agent modified ultrafine calcium carbonate filler |
| CN104479415A (en) * | 2014-12-26 | 2015-04-01 | 天津滨浦生产力促进有限公司 | Calcium carbonate surface modifier |
| CN105504891A (en) * | 2015-12-06 | 2016-04-20 | 天津儒创新材料科技有限公司 | Preparation method of rare earth modifier |
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