CN103804953A - Method for preparing ultrafine surface modified dolomite - Google Patents
Method for preparing ultrafine surface modified dolomite Download PDFInfo
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- CN103804953A CN103804953A CN201310664396.5A CN201310664396A CN103804953A CN 103804953 A CN103804953 A CN 103804953A CN 201310664396 A CN201310664396 A CN 201310664396A CN 103804953 A CN103804953 A CN 103804953A
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Abstract
The invention discloses a method for preparing ultrafine surface modified dolomite, which is a method for preparing ultrafine modified dolomite by using mechanical chemical method. According to the method, dolomite is crushed, and then is added into a ball mill to obtain ultrafine modified dolomite powder through modifying agent based on dry ball milling. The method is a method for crushing dolomite into ultrafine powder and simultaneously surface modifying, the method not only simplifies the production process but also the product obtained according to the method has fine size and is centralized in distribution, and meanwhile the physical-chemical properties of the surface of dolomite powder are improved, the compatibility between dolomite powder and matrix is enhanced, and better mechanical strength and mechanical property of the material are kept.
Description
Technical field
The present invention relates to a kind of preparation method of superfine modified rhombspar, relate to specifically the object that reaches surface modification when a kind of mechanochemical method makes rhombspar super-refinement.
Background technology
Rhombspar is a kind of common white nonmetal mineral thing, belongs to CaCO
3and MgCO
3compound carbonate mineral, extremely abundant in China's standing stock, be a kind of important calcium magnesium resource.Rhombspar has been widely used in the industries such as plastics, rubber, binding agent as filler.But oarse-grained rhombspar powder can cause that in macromolecular material the physical strength of material itself is as the deterioration of the indices such as stretch-proof ability and elongation at break, rhombspar super-refinement is become a kind of inevitable.
At present, physical pulverization method relies on its cost advantage low, that production technique is simple and output is large to become production superfine powdery material method the most widely.The research of super-pine crush equipment using mainly contains micronizer mill, mechanical shock pulverizer, ball mill, vibration mill, stirring mill, colloidal mill etc.The product of pulverizing out is because fine size, narrowly distributing, quality are even, thereby have that specific surface area is large, surfactivity is high, chemical reaction velocity is fast, dissolution rate is fast, sintered compact intensity is large and unique electrically, magnetic, optical etc., thereby be widely used in many technical fields.But, because having small-size effect, surface and interface effect, macro quanta tunnel effect, superfine powder make it be easy to reunite, be difficult for disperseing in organic medium, and poor with matrix compatibility, directly affect its actual effect.One of the most effective approach that superfine powder is carried out to dispersion treatment carries out surface modification to it exactly, thus reach improve powder physicochemical property, reinforcing filler and matrix consistency, improve dispersed, improve interfacial property, give the object of the new function of particle.
At present, powder being carried out to surface modification mainly contains surface coverage modification, topochemistry modification, mechanical-chemical modification, outer membrane modification, high-energy surface modification and utilizes precipitin reaction to carry out surface modification etc.Mechanical-chemical modification refers to by means such as compression, shearing, friction, extension, bending, impacts, and material is applied to mechanical energy, thereby the physicochemical property of bringing out material change, the method that itself and material are around reacted.In changing the surface properties of the natural hydrophilic oleophobic of product, improve its consistency in polymkeric substance, reduce its impact on polymeric articles processing characteristics and mechanical property, even make their over-all propertieies increase.
Past technological achievement shows according to this, first rhombspar is roughly ground, and afterwards it is carried out to mechanical-chemical modification, although the product obtaining is good with macromolecular material consistency, but exists the shortcoming that powder granularity is thin not; And first by rhombspar superfine grinding, then it is carried out wet-process modified, exist that complex manufacturing, properties-correcting agent and powder surface affinity are poor, the weak and inhomogeneous shortcoming of adhewsive action.
Summary of the invention
For the deficiency of above-mentioned technology, the present invention proposes the technology that a kind of preparation method of super fine bitter spar, a kind of mechanical force and chemical method prepare superfine modified rhombspar, when being carried out to superfine grinding, powder completes the surface active modification of powder.Technical process of the present invention is first rhombspar to be pulverized and made rhombspar powder, and then makes superfine modified powder through properties-correcting agent dry ball milling in ball mill; Concrete technical scheme realizes as follows:
1) rhombspar is pulverized and obtained the rhombspar powder that size is 4-7um;
2) rhombspar powder step 1) being obtained joins in the ball grinder of ball mill, then adding quality is the properties-correcting agent of powder quality 1.5%-5%, be that 200-500r/min, temperature are under the condition of 60-90 ℃ at rotational speed of ball-mill, dry ball milling 100-120min obtains the super fine bitter spar powder of surface modification, and the grinding medium in ball mill is abrading-ball.
Preferably, in the present invention the rhombspar powder described in step 1) obtains with airflow milling fine grinding after Raymond machine corase grind.
Preferably, step 2) described in the number of abrading-ball be 20-60, diameter is between 5mm-10mm, the ratio that abrading-ball is 15-25 in ratio of grinding media to material adds.
Preferably, step 2 in the present invention) described abrading-ball be two kinds of different sizes abrading-ball mix, be of a size of any two numerical value of diameter between 5mm-10mm, the number of described abrading-ball is any two numerical value between 10-30, the abrading-ball that can be also multiple different size mixes, and the ratio that abrading-ball is 15-25 in ratio of grinding media to material adds.
Preferably, in the present invention described abrading-ball is aluminum oxide or zirconium white.
Preferably, step 2 in the present invention) described ball mill is planetary ball mill, thereby this principle of variation induction physicochemical change that the present invention utilizes solid material that form, crystalline structure can occur under mechanical force is produced superfine powdery material, and planetary ball mill advantage is to make full use of mechanical force and chemical and acts on and when carrying out superfine grinding, carry out surface active modification.
Preferably, in the present invention step 2) described in properties-correcting agent be higher fatty acid, higher fatty acid salt or coupling agent.
Preferably, in the present invention the carbonatoms of described higher fatty acid, higher fatty acid salt is between 16-18.
Preferably, in the present invention described coupling agent is titanate coupling agent, boric acid ester coupler, silane coupling agent, aluminum-zirconium coupling agent, aluminate coupling agent, aluminium titanium composite coupler or aluminium zirconium composite coupler.
Step 2 in the present invention) the super fine bitter spar powder median size D50 of described surface modification is 1.0um.
Step 2 in the present invention) described in the super fine bitter spar powder particle diameter D97 of surface modification be 2.0um.
The quality of product modified effect embodies by activation rate, the specific experiment process of activation rate test is as follows: accurately take sample after 1g modification in 20ml graduated cylinder, add water to 15ml, vibration shakes up rear standing 30min, at this moment a powder part for modification floats on the upper strata of water, a part sinks to the bottom, reads floating volume and the sinking volume of sample after kept in balance;
V1: floating volume;
V2: sinking volume;
The larger explanation surface modification effect of degree of activation is better, and what it more embodied is the ratio of modification.Unmodified rhombspar surface presents the characteristic of hydrophilic oleophobic, and it is carried out to surface modification is the consistency in order to increase itself and organic phase, thereby when making it give full play to filler effect, does not change the mechanical property of material.
In order further to verify the consistency of modification dolomite and organic phase, respectively modification and unmodified rhombspar are carried out to oil absorbency mensuration, relatively the variation of both oil absorbencies.Detailed process is as follows: take respectively 5g modification and unmodified rhombspar powder on watch-glass, limit is stirred limit drop-burette with glass stick and dripped Viscotrol C, records the consumption of Viscotrol C in the time that powder is just bonded to pelletizing.
Oil absorbency formula: oil absorbency=Viscotrol C consumption/powder consumption
Mechanics Performance Testing: by PP(polypropylene) mix in different ratios from rhombspar, on double roller plastic-making device, melting is compound, mixing even rear tab is taken off, after hot-forming on vulcanizing press, take off in chilling press pressurize cooling, take out cutting sample preparation, it is carried out to tensile property and impact property test.
Beneficial effect of the present invention: a kind of technological method that the superfine grinding of rhombspar powder and surface modification are carried out is simultaneously provided, simplify production technique, the product granularity that obtains is thin, distribute and concentrate, improve the physicochemical property of ground dolomite surface, when strengthening the consistency between rhombspar powder and matrix, kept the good physical strength of material and mechanical property.
accompanying drawing explanationthe preparation method of the ultra-fine surface modification rhombspar of Fig. 1.
Embodiment
Embodiment 1:
In the ball grinder of planetary ball mill, adding particle diameter is the rhombspar powder of 5 um, take rhombspar as 100 weight parts, adds the stearic acid of 2 deals, ball milling 100min at 60 ℃, and obtaining particle diameter described in the invention is the modification dolomite powder of 2um; Sample degree of activation is 99.3% after testing; Modification dolomite powder has reduced 12.5% than unmodified ground dolomite oil absorbency; The rhombspar of long time without surface modification joins in PP, declines gradually with the increase tensile strength of content, and when after modification, rhombspar loading level reaches 2%, tensile strength maximum; The rhombspar of non-modified joins in PP, and goods impact property reaches maximum 6.5 MPa 1%, and after stearic acid modified, matrix material impact property in the time that modification dolomite loading level is 2% is up to 6.8 MPa.
Embodiment 2:
In the ball grinder of planetary ball mill, adding particle diameter is the rhombspar powder of 6 um, take rhombspar as 100 weight parts, adds the stearate of 2 deals, ball milling 100 min at 75 ℃, and obtaining particle diameter described in the invention is the modification dolomite powder of 2 um; Sample degree of activation is 99.5% after testing; Modification dolomite powder has reduced 13.8% than unmodified ground dolomite oil absorbency; After modification, rhombspar joins in PP, when loading level reaches 3%, and tensile strength maximum; After stearate modification, matrix material impact property in the time that modification dolomite loading level is 3% is up to 7.0 MPa.
Embodiment 3:
In the ball grinder of planetary ball mill, adding particle diameter is the rhombspar powder of 7 um, take rhombspar as 100 weight parts, add the silane coupling agent of 2.5 deals, ball milling 120 min at 80 ℃, obtaining particle diameter described in the invention is the modification dolomite powder of 2 um; Sample degree of activation is 99.1% after testing; Modification dolomite powder has reduced 12.3% than unmodified ground dolomite oil absorbency; After modification, rhombspar joins in PP, when loading level reaches 3%, and tensile strength maximum; After silane coupling agent surface modification, matrix material impact property in the time that modification dolomite loading level is 3% is up to 7.0 MPa.
Embodiment 4:
In the ball grinder of planetary ball mill, adding particle diameter is the rhombspar powder of 4 um, take rhombspar as 100 weight parts, add the titanate coupling agent of 5 deals, ball milling 120 min at 80 ℃, obtaining particle diameter described in the invention is the modification dolomite powder of 2 um.Sample degree of activation is 99.6% after testing; Modification dolomite powder has reduced 13.9% than unmodified ground dolomite oil absorbency; After modification, rhombspar joins in PP, when loading level reaches 3%, and tensile strength maximum; After titanate coupling agent surface modification, matrix material impact property in the time that modification dolomite loading level is 3% is up to 7.2MPa.
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; any be familiar with those skilled in the art the present invention disclose technical scope in; be equal to replacement or changed according to technical scheme of the present invention and inventive concept thereof, within all should being encompassed in protection scope of the present invention.
Claims (10)
1. the preparation method of ultra-fine surface modification rhombspar, is characterized in that, comprise the steps,
1) rhombspar is pulverized and obtained the rhombspar powder that size is 4-7um;
2) rhombspar powder step 1) being obtained joins in the ball grinder of ball mill, then adding quality is the properties-correcting agent of powder quality 1.5%-5%, be that 200-500r/min, temperature are under the condition of 60-90 ℃ at rotational speed of ball-mill, dry ball milling 100-120min obtains the super fine bitter spar powder of surface modification, and the grinding medium in ball mill is abrading-ball.
2. the preparation method of ultra-fine surface modification rhombspar according to claim 1, is characterized in that, the rhombspar powder described in step 1) obtains with airflow milling fine grinding after roughly grinding by Raymond machine.
3. the preparation method of ultra-fine surface modification rhombspar according to claim 1, is characterized in that step 2) described in the number of abrading-ball be 20-60, diameter is between 5mm-10mm, the ratio that abrading-ball is 15-25 in ratio of grinding media to material adds.
4. the preparation method of ultra-fine surface modification rhombspar according to claim 1, it is characterized in that, step 2) described in abrading-ball be two kinds of different sizes abrading-ball mix, be of a size of any two numerical value of diameter between 5mm-10mm, the number of described abrading-ball is any two numerical value between 10-30, and the ratio that abrading-ball is 15-25 in ratio of grinding media to material adds.
5. according to the preparation method of the ultra-fine surface modification rhombspar described in claim 1,3 or 4, it is characterized in that, described abrading-ball is aluminum oxide or zirconium white.
6. the preparation method of ultra-fine surface modification rhombspar according to claim 1, is characterized in that step 2) described ball mill is planetary ball mill.
7. the preparation method of ultra-fine surface modification rhombspar according to claim 1, is characterized in that step 2) described in properties-correcting agent be higher fatty acid, higher fatty acid salt or coupling agent.
8. the preparation method of ultra-fine surface modification rhombspar according to claim 7, is characterized in that, the carbonatoms of described higher fatty acid, higher fatty acid salt is between 16-18.
9. the preparation method of ultra-fine surface modification rhombspar according to claim 7, it is characterized in that, described coupling agent is titanate coupling agent, boric acid ester coupler, silane coupling agent, aluminum-zirconium coupling agent, aluminate coupling agent, aluminium titanium composite coupler or aluminium zirconium composite coupler.
10. the preparation method of ultra-fine surface modification rhombspar according to claim 1, is characterized in that step 2) described in the particle diameter D50 of super fine bitter spar powder of surface modification be 1.0um, D97 is 2.0um.
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Cited By (8)
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CN105542251A (en) * | 2016-01-20 | 2016-05-04 | 苏州市景荣科技有限公司 | Foamed composite rubber shoe sole material and preparation method thereof |
CN107418250A (en) * | 2017-08-10 | 2017-12-01 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of modification dolomite |
CN109988912A (en) * | 2019-05-20 | 2019-07-09 | 济南鸿泰华丰机械有限公司 | A kind of resource utilization method of landfill leachate |
CN111111890A (en) * | 2019-11-21 | 2020-05-08 | 乐山爬吸道休闲健身服务部 | Preparation method of rock salt small granules for treating respiratory diseases |
CN111234565A (en) * | 2020-03-16 | 2020-06-05 | 库车塔北泥浆材料有限公司 | Modification method of activated barite powder |
CN111334090A (en) * | 2020-02-26 | 2020-06-26 | 上海应用技术大学 | Modified fly ash and preparation method thereof |
CN113025077A (en) * | 2021-03-01 | 2021-06-25 | 武宣宝丰矿业有限公司 | Preparation method of superfine dolomite powder |
CN113136108A (en) * | 2021-04-02 | 2021-07-20 | 湖北工业大学 | Preparation method of superfine inorganic micro powder modified asphalt |
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CN105542251A (en) * | 2016-01-20 | 2016-05-04 | 苏州市景荣科技有限公司 | Foamed composite rubber shoe sole material and preparation method thereof |
CN105542251B (en) * | 2016-01-20 | 2017-10-20 | 广州市欧橡隔热材料有限公司 | One kind foaming compounded rubber material for sole of shoe and preparation method thereof |
CN107418250A (en) * | 2017-08-10 | 2017-12-01 | 青阳县永诚钙业有限责任公司 | A kind of preparation method of modification dolomite |
CN109988912A (en) * | 2019-05-20 | 2019-07-09 | 济南鸿泰华丰机械有限公司 | A kind of resource utilization method of landfill leachate |
CN109988912B (en) * | 2019-05-20 | 2020-05-05 | 鸿灌环境技术有限公司 | Resource utilization method of landfill leachate |
CN111111890A (en) * | 2019-11-21 | 2020-05-08 | 乐山爬吸道休闲健身服务部 | Preparation method of rock salt small granules for treating respiratory diseases |
CN111334090A (en) * | 2020-02-26 | 2020-06-26 | 上海应用技术大学 | Modified fly ash and preparation method thereof |
CN111234565A (en) * | 2020-03-16 | 2020-06-05 | 库车塔北泥浆材料有限公司 | Modification method of activated barite powder |
CN113025077A (en) * | 2021-03-01 | 2021-06-25 | 武宣宝丰矿业有限公司 | Preparation method of superfine dolomite powder |
CN113136108A (en) * | 2021-04-02 | 2021-07-20 | 湖北工业大学 | Preparation method of superfine inorganic micro powder modified asphalt |
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Effective date of registration: 20180511 Address after: 118200 B6 block, Qing Yishan Industrial Park, Kuandian Manchu Autonomous County, Dandong, Liaoning Patentee after: Dandan Yilong High-Tech Material Co., Ltd. Address before: 116001 No. 11, 1 unit 11, Lu Xun Road, Zhongshan District, Dalian, Liaoning, No. 1, No. 11 Patentee before: LIAONING YILONG MINING CO., LTD. |