CN102134405A - Preparation method of superfine inorganic powder for filling polypropylene - Google Patents
Preparation method of superfine inorganic powder for filling polypropylene Download PDFInfo
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- CN102134405A CN102134405A CN2010106001692A CN201010600169A CN102134405A CN 102134405 A CN102134405 A CN 102134405A CN 2010106001692 A CN2010106001692 A CN 2010106001692A CN 201010600169 A CN201010600169 A CN 201010600169A CN 102134405 A CN102134405 A CN 102134405A
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Abstract
The invention relates to a preparation method of superfine talcum powder for filling polypropylene, which is characterized by being prepared by the following steps of: adding water into the talcum powder to prepare into a disperse liquid; adding 1-2% of coupling agent or reactive monomers based on the weight of the talcum powder into the disperse liquid for wet grinding, wherein 0.4-1.0mm zirconium oxide beads serve as grinding media; and drying the material in vacuum after the grinding is completed and water is removed through standing. In the invention, the superfine crushing and the surface modification of the talcum powder are integrated, and the modification effect is obvious; and compared with the filling results of unmodified powder, the superfine talcum powder has higher strength and rigidity, the impact strength of the superfine talcum powder is greatly improved, and meanwhile, the whiteness of the powder and filling products is improved.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic powder, particularly relate to the preparation method of a kind of filled polypropylene with ultrafine inorganic powder.
Background technology
Talcum powder as modal silicate mine, is a kind of good filler for plastic.But talcum powder belongs to polarity, water-insoluble substance, when it is dispersed in the little plastics of polarity, because of polarity difference, can cause both consistencies not good.Therefore its surface is suitably handled very and be necessary.Generally, can make its surface polarity near the polymkeric substance of being filled, perhaps make its surface have the functional group of reactable, thereby improve the interface in conjunction with effect by chemical reaction or physical method.
Usually, in polymer processing, be chosen in mostly and carry out the dry method coating processing in the high-speed mixer.Use KH-550 silane coupling agent, sodium stearate surface modification talcum powder.This method is simple.But only play the effect of powder surface modification.Use the ultra-fine vibration mill abrasive inorganic of cartridge type powder, and use surface-modifying agent is sprayed onto powder surface, realize superfine modified integrated.The particle diameter that this method obtains is still bigger, the particle diameter of 15～20 μ m, the follow-up stage treatment that needs.And the dry process environmental pollution is bigger.
Document has been told about the surface treatment method of a kind of oxide powder, oxyhydroxide powder, clay mineral powder, carbonate powder.Adopt water and organic solvent two-phase interface and phase transition, in non-polar solvent, inorganic particulate is carried out surface chemical modification.This method adopts benzene kind solvent, and step is numerous and diverse, and does not set forth modified effect.
The present invention is directed to above deficiency,, make talcous superfine grinding and surface modification integrated, and modified effect is remarkable with the method for simple and feasible environmental protection.Powder filled result with non-modified compares, and has higher intensity and rigidity, and shock strength increases substantially, and simultaneously, the whiteness of powder and filled articles is improved.
Summary of the invention
The purpose of this invention is to provide a kind of new talcum powder superfine grinding and the method for surface modification.By high energy milling, shearing impact constantly takes place, and the inorganic particulate surface constantly generates new interface, and coupling agent or reactive monomer fully contact with inorganic powder surface, reaches certain physical and chemical effect takes place under good dispersion state, can significantly improve the effect of modification.Specifically be described below:
The invention provides the preparation method of a kind of filled polypropylene with ultrafine inorganic powder, it is characterized in that, add water with talcum powder, be mixed with dispersion liquid, add the coupling agent or the reactive monomer that account for talcum powder weight 1～2%, carry out wet grinding, grinding medium is the zirconium white zirconium pearl of 0.4mm～1.0mm, grinding finishes, display anhydrate after, vacuum drying makes the filled polypropylene superfine talcum powder.
Described coupling agent is a silane coupling agent; Reactive monomer is vinylformic acid or methacrylic acid or carboxylate salt.
Described wet grinding is in a sealed cylinder block, adds the grinding medium of cylinder body long-pending 70%, agitation grinding medium, shearing impact talcum powder.
Described talcum powder granularity is 4325～1250 orders; Described dispersion liquid concentration is 100～300g/L.
Description of drawings
Former talcum powder of Fig. 1 and the talcum powder size distribution contrast of processing back
The former talcum powder SEM figure of Fig. 2
Talcous SEM figure after Fig. 3 embodiment 1 handles
Talcous infared spectrum after Fig. 4 embodiment 1 handles
Embodiment
Further specify the present invention below by embodiment and Comparative Examples, do not violating under the aim condition of the present invention, the present invention should be not limited to following experimental example and specifically express content.
Add water with 800 order talcum powder, be mixed with the dispersion liquid of 150g/L concentration.Add the silane coupling agent γ-methacryloxypropyl trimethoxy silane (KH-570) that accounts for talcum powder weight 1.2%, carry out wet grinding with DMQ wet grinding machine,, grinding medium is the zirconium white zirconium pearl of 0.4mm, the grinding rotating speed is 3375rpm, and the time is 2h.Grinding finishes, display anhydrate after, vacuum drying is pulverized, prepared talcum powder and former talcous infrared spectra are shown in figure four.From infrared spectra as can be seen, through after wet grinding and the surface modification, at 1450cm
-1And 880cm
-1The peak at place becomes more sharp-pointed.With 1003cm
-1The peak at place is that the stretching vibration peak of Si-O-Si is a benchmark, calculates 1450cm
-1The place changes, former talcum powder I
1450/ I
1003=0.159, the talcum powder I after the processing
1450/ I
1003=0.646, tentatively infer 1450cm
-1The peak is CO
3 2-Antisymmetric stretching vibration, 880cm
-1Be CO
3 2-Flexural vibration.Illustrate in the wet grinding process CO is arranged
3 2-Generate.
Size-grade distribution is as shown in table 1.
Whiteness is through the test of WSB-3 blancometer, and former talcum powder whiteness is 48.88wb, and the talcum powder whiteness of gained is 52.60wb after the wet grinding modification.
The powder that makes is joined among the PP, basic ratio is a talcum powder: polypropylene: polyethylene octene elastomer=20: 75: 5, and whiteruss helps mixed, and twin screw extruder is extruded pelletizing, the processing temperature scope is 180-215 ℃, and the twin screw rotating speed is 180 commentaries on classics/min.The test of injection moulding standard batten, performance test is carried out according to every standard of table 2.
The former talcum powder of table 1 and handled talcum powder particle diameter contrast
| d(0.1) | d(0.5) | D(0.9) | |
| Former talcum powder | 3.210 | 12.657 | 39.866 |
| Handle the back talcum powder | 2.266 | 6.634 | 16.418 |
Embodiment 2
Add water with 800 order talcum powder, be mixed with the dispersion liquid of 150g/L concentration.Add the vinylformic acid (AA) that accounts for talcum powder weight 2%, carry out wet grinding with DMQ wet grinding machine, grinding medium is the zirconium white zirconium pearl of 0.4mm, and the grinding rotating speed is 3375rpm, and the time is 2h.Grinding finishes, display anhydrate after, vacuum drying is pulverized, size-grade distribution is as shown in table 2.
Whiteness is through the test of WSB-3 blancometer, and former talcum powder whiteness is 48.88wb, and the talcum powder whiteness of gained is 50.20wb after the modification.
The powder that makes is joined among the PP, basic ratio is a talcum powder: polypropylene: polyethylene octene elastomer=20: 75: 5, whiteruss helps mixed, add anti ultraviolet agent and antioxidant simultaneously, twin screw extruder is extruded pelletizing, the processing temperature scope is 180-215 ℃, and the twin screw rotating speed is 180 commentaries on classics/min.The test of injection moulding standard batten, performance test is carried out according to every standard of table 2.
Former talcum powder of table 2 and AA handled the contrast of talcum powder particle diameter
| d(0.1) | d(0.5) | D(0.9) | |
| Former talcum powder | 3.210 | 12.657 | 39.866 |
| AA handles the back talcum powder | 1.937 | 6.040 | 16.467 |
Comparative Examples 1
Join among the PP with 800 order talcum powder, basic ratio is a talcum powder: polypropylene: polyethylene octene elastomer=20: 75: 5, and whiteruss helps mixed, and twin screw extruder is extruded pelletizing, the processing temperature scope is 180-215 ℃, and the twin screw rotating speed is 180 commentaries on classics/min.The test of injection moulding standard batten, performance test is carried out according to every standard of table 2, and the test result contrast is as shown in table 3.
Comparative Examples 2
Add water with 800 order talcum powder, be mixed with the dispersion liquid of 150g/L concentration, carry out wet grinding with DMQ wet grinding machine, grinding medium is the zirconium white zirconium pearl of 0.4mm, and the grinding rotating speed is 3375rpm, and the time is 2h.Grinding finishes, display anhydrate after, vacuum drying, pulverize, the powder that makes is joined among the PP, basic ratio is a talcum powder: polypropylene: polyethylene octene elastomer=20: 75: 5, whiteruss helps mixed, twin screw extruder is extruded pelletizing, and the processing temperature scope is 180-215 ℃, and the twin screw rotating speed is 180 commentaries on classics/min.The test of injection moulding standard batten, performance test is carried out according to every standard of table 2.The test result contrast is as shown in table 3.
As shown in Table 3, the performance of the filling-modified PP of talcum powder after wet grinding is handled all is better than former talcum powder basically.With reference to Comparative Examples 2 and embodiment as can be seen, in wet grinding, carry out surface modification, rigidity can slightly descend, and erosion-resisting characteristics but increases substantially, and especially the shock strength under the normal temperature improves about 70%.
Each performance test reference standard tabulation of table 3
| Project | Standard |
| Tensile strength | GB/T 1040-2006, speed 50mm/min |
| Tensile modulus | GB/T?1040-2006 |
| Flexural strength | GB/T 9341-2000, speed 2mm/min |
| Modulus in flexure | GB/T?9341-2000 |
| MFR | GB/T?3682-2000，230℃，2.16kg |
| Cantilever beam impact strength | GB/T?1043.1-2008 |
| Whiteness | GB/T?2913-1982 |
Table 4 The performance test results tabulation (23 ℃, 50%)
Claims (4)
1. a filled polypropylene is with the preparation method of ultrafine inorganic powder, it is characterized in that, add water with talcum powder, be mixed with dispersion liquid, add the coupling agent or the reactive monomer that account for talcum powder weight 1～2%, carry out wet grinding, grinding medium is the zirconium white zirconium pearl of 0.4mm～1.0mm, grinding finishes, display anhydrate after, vacuum drying makes the filled polypropylene superfine talcum powder.
2. a kind of filled polypropylene according to claim 1 is characterized in that with the preparation method of ultrafine inorganic powder described coupling agent is a silane coupling agent; Reactive monomer is vinylformic acid or methacrylic acid or carboxylate salt.
3. a kind of filled polypropylene according to claim 1 is characterized in that with the preparation method of ultrafine inorganic powder described wet grinding is in a sealed cylinder block, adds the grinding medium of cylinder body long-pending 70%, agitation grinding medium, shearing impact talcum powder.
4. a kind of filled polypropylene according to claim 1 is characterized in that with the preparation method of ultrafine inorganic powder described talcum powder granularity is 4325～1250 orders; Described dispersion liquid concentration is 100～300g/L.
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| CN2010106001692A CN102134405A (en) | 2010-12-21 | 2010-12-21 | Preparation method of superfine inorganic powder for filling polypropylene |
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| CN2010106001692A CN102134405A (en) | 2010-12-21 | 2010-12-21 | Preparation method of superfine inorganic powder for filling polypropylene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275522A (en) * | 2013-06-13 | 2013-09-04 | 南宝树脂（中国）有限公司 | Method for preparing silane coupling agent cladding modified talcum powder and silver mirror back coating |
| CN112442289A (en) * | 2020-11-10 | 2021-03-05 | 桂林桂广申巴粉体材料有限责任公司 | Modified talcum powder, and preparation method and application thereof |
| CN114702726A (en) * | 2022-04-13 | 2022-07-05 | 广西科学院 | Preparation method of superfine active talcum powder special for polypropylene plastic for vehicle |
-
2010
- 2010-12-21 CN CN2010106001692A patent/CN102134405A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103275522A (en) * | 2013-06-13 | 2013-09-04 | 南宝树脂（中国）有限公司 | Method for preparing silane coupling agent cladding modified talcum powder and silver mirror back coating |
| CN103275522B (en) * | 2013-06-13 | 2014-10-01 | 南宝树脂（中国）有限公司 | Method for preparing silane coupling agent cladding modified talcum powder and silver mirror back coating |
| CN112442289A (en) * | 2020-11-10 | 2021-03-05 | 桂林桂广申巴粉体材料有限责任公司 | Modified talcum powder, and preparation method and application thereof |
| CN112442289B (en) * | 2020-11-10 | 2021-09-14 | 桂林桂广申巴粉体材料有限责任公司 | Modified talcum powder, and preparation method and application thereof |
| CN114702726A (en) * | 2022-04-13 | 2022-07-05 | 广西科学院 | Preparation method of superfine active talcum powder special for polypropylene plastic for vehicle |
| CN114702726B (en) * | 2022-04-13 | 2024-02-13 | 广西科学院 | Preparation method of special superfine active talcum powder for automotive polypropylene plastic |
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Application publication date: 20110727 |