CN103275473A - Modified feldspar, polylactic acid-modified feldspar composite material, and preparation method and product thereof - Google Patents
Modified feldspar, polylactic acid-modified feldspar composite material, and preparation method and product thereof Download PDFInfo
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Abstract
The invention relates to modified feldspar, a polylactic acid-modified feldspar composite material, and a preparation method thereof. The polylactic acid-modified feldspar composite material comprises a polylactic acid resin, the modified feldspar, a nucleating agent and a plasticizer. The polylactic acid-modified feldspar composite material is obtained by the following steps of mixing the polylactic acid resin, the modified feldspar, the nucleating agent and the plasticizer according to required amounts thoroughly and uniformly by using a stirring mixer, and then introducing the above mixture to a single screw extruder to carry out extrusion. The obtained modified feldspar has a large interface contact angle and reduced surface hydrophily (enhanced surface lipophilicity), enabling the surface of the feldspar to realize organization modification, to form good interface compatibility with a polylactic acid matrix and to form good dispersibility at the interface. The polylactic acid-modified feldspar composite material obtained by the modified feldspar has significantly enhanced mechanical property, heat stability and toughness, so that application fields of the polylactic acid is broadened and the polylactic acid-modified feldspar composite material has great application prospects.
Description
Technical field
The present invention relates to the lactic acid composite material technical field, is a kind of modification feldspar, polylactic acid-modified feldspar matrix material and preparation method thereof and goods.
Background technology
(Polylactic acid, PLA) macromolecular material not only can natural degradation in physical environment, and can degrade nontoxic and good biocompatibility in vivo for poly(lactic acid).Be widely used mainly as tissue engineering bracket material, medicine control slow-release material etc. at present.Compare with conventional plastic, it is carbonic acid gas and water that poly(lactic acid) is burned after product, and the carbonic acid gas of generation can be by plant absorbing, and the photosynthesis of involved in plant can not cause carrying capacity of environment, is a kind of environmentally friendly macromolecular material.Because the poly(lactic acid) crystallization velocity slowly causes poly(lactic acid) to have fatal defective: matter is crisp, thermostability is relatively poor, shock resistance is relatively poor, poor toughness etc.Therefore its Application Areas is restricted.In order to overcome these defectives of poly(lactic acid), it is material modified to carry out composite modified preparation to poly(lactic acid), thereby expands its Application Areas.
At present, adopting montmorillonite carries out modification to poly(lactic acid) and prepares nano composite polymer/laminated silicate material (Polymer/Layered Silicate Nanocomposite, PLSN) as an important branch of polylactic acid modified composite material and be widely studied, although polynite can improve the thermostability of poly(lactic acid), but to begin the anisotropy hydrolysis after the PLA suction be that major cause that the degraded of PLA nano composite material is accelerated (sees public publication for details: Sinha R S because the oh group of polynite terminal makes, Yamada K, Okamoto M, et al. New polylactide/ layered silicate nanocomposites: 5. Designing of materials with desired properties. Polymer, 2003,44 (21): 6633-6646.), thereby reduced the mechanical property of PLA material.Glass fibre can strengthen the mechanical property of poly(lactic acid), but since the hold-time of the relatively poor intensity that causes poly-lactic acid material of the interface compatibility between glass fibre and the poly(lactic acid) and modulus shortly (see public publication for details: Steve T L Wuhan International Synposium on Biomaterials and Fine Polymers.1994:50).Adopt charcoal fiber, the compound enhancing poly(lactic acid) of natural fiber, because it is acid that the poly(lactic acid) degraded product is, easily cause inflammatory reaction in the body, the application of charcoal fiber reinforcement poly(lactic acid) is restricted and (sees public publication: Shen Lie for details, Qiao Fei, Zhang Yuqiang etc., mechanical property and the external degradation performance of charcoal fiber reinforcement hydroxylapatite/polylactic acid composite biological material, the matrix material journal, 2007,24 (5): 61-65).
Summary of the invention
The invention provides a kind of modification feldspar, polylactic acid-modified feldspar matrix material and preparation method thereof and goods, overcome the deficiency of above-mentioned prior art; By modification the surface hydrophilicity of feldspar being weakened is that surperficial lipophilicity strengthens, make the feldspar surface realize organic modification, thereby improve interface compatibility and interface dispersiveness between modification feldspar and the poly(lactic acid) matrix, further improve mechanical property, shock resistance, toughness and the thermostability of lactic acid composite material, thereby expanded the Application Areas of poly(lactic acid).
One of technical scheme of the present invention realizes by following measure:
A kind of modification feldspar obtains by following step: the first step, getting an amount of Feldspar Powder, to be broken to particle diameter be 60 microns to 74 microns Feldspar Powder, Feldspar Powder after the pulverizing adds in the dehydrated alcohol and stirs, obtain Feldspar Powder suspension after stirring, the mass percent concentration of Feldspar Powder in Feldspar Powder suspension is 5% to 30%; Second step, join 0.5 gram to 10 gram properties-correcting agent by 100 gram feldspars and take by weighing properties-correcting agent, it is to be made into the properties-correcting agent hydrolyzed solution in 50% to 90% the ethanolic soln that the properties-correcting agent that takes by weighing is dissolved in concentration of volume percent, the mass percent concentration of properties-correcting agent in the properties-correcting agent hydrolyzed solution is 16.7% to 50%, the Feldspar Powder suspension that the first step is obtained joins in the properties-correcting agent hydrolyzed solution and is stirred into mixed solution, regulate the pH value to 3.5 of mixed solution, mixed solution hydrolysis after the adjusting pH value places it in the microwave reactor after 30 minutes to 120 minutes, is that microwave exposure obtains modification feldspar slurry under 20 W to 50W after 20 minutes to 60 minutes at power; The 3rd step, modification feldspar slurry is filtered, obtain the modification feldspar after the filter cake drying after the filtration, the pulverizing.
Be the further optimization and/or improvements to one of foregoing invention technical scheme below:
In the above-mentioned the first step, the Feldspar Powder after will pulverizing adds in the dehydrated alcohol and stirs, and stirring velocity is that 400 rev/mins to 2000 rev/mins, churning time are 30 minutes to 60 minutes, obtains Feldspar Powder suspension after the stirring; Or/and, the 3rd step, modification feldspar slurry is filtered, the filter cake after the filtration is 100 ℃ to 105 ℃ down after dry 2 hours to 3 hours in temperature, is ground into particle diameter and is 60 microns to 74 microns to obtain the modification feldspar; Or/and properties-correcting agent is more than one mixtures in silane coupling agent, titanate coupling agent and the aluminate coupling agent.
Two of technical scheme of the present invention realizes by following measure: a kind of preparation method of modification feldspar is undertaken by following step: the first step, getting an amount of Feldspar Powder, to be broken to particle diameter be 60 microns to 74 microns Feldspar Powder, Feldspar Powder after the pulverizing adds in the dehydrated alcohol and stirs, obtain Feldspar Powder suspension after stirring, the mass percent concentration of Feldspar Powder in Feldspar Powder suspension is 5% to 30%; Second step, join 0.5 gram to 10 gram properties-correcting agent by 100 gram feldspars and take by weighing properties-correcting agent, it is to be made into the properties-correcting agent hydrolyzed solution in 50% to 90% the ethanolic soln that the properties-correcting agent that takes by weighing is dissolved in concentration of volume percent, the mass percent concentration of properties-correcting agent in the properties-correcting agent hydrolyzed solution is 16.7% to 50%, the Feldspar Powder suspension that the first step is obtained joins in the properties-correcting agent hydrolyzed solution and is stirred into mixed solution, regulate the pH value to 3.5 of mixed solution, mixed solution hydrolysis after the adjusting pH value places it in the microwave reactor after 30 minutes to 120 minutes, is that microwave exposure obtains modification feldspar slurry under 20 W to 50W after 20 minutes to 60 minutes at power; The 3rd step, modification feldspar slurry is filtered, obtain the modification feldspar after the filter cake drying after the filtration, the pulverizing.
Be two further optimization and/or improvements to the foregoing invention technical scheme below:
In the above-mentioned the first step, the Feldspar Powder after will pulverizing adds in the dehydrated alcohol and stirs, and stirring velocity is that 400 rev/mins to 2000 rev/mins, churning time are 30 minutes to 60 minutes, obtains Feldspar Powder suspension after the stirring; Or/and, the 3rd step, modification feldspar slurry is filtered, the filter cake after the filtration is 100 ℃ to 105 ℃ down after dry 2 hours to 3 hours in temperature, is ground into particle diameter and is 60 microns to 74 microns to obtain the modification feldspar; Or/and properties-correcting agent is more than one mixtures in silane coupling agent, titanate coupling agent and the aluminate coupling agent.
Three of technical scheme of the present invention realizes by following measure: a kind of polylactic acid-modified feldspar matrix material that uses the modification feldspar, and raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Be three further optimization and/or improvements to the foregoing invention technical scheme below:
The polylactic acid-modified feldspar matrix material of above-mentioned use modification feldspar, raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 0.1 part to 1 part of nucleator, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature; Or/and nucleator is more than one mixtures in talcum powder, carbon nanotube, calcium carbonate, clay and the amides; Or/and softening agent is more than one mixtures in polyoxyethylene glycol, organic acid acetic, phosphoric acid ester, polyester and the tributyl acetylcitrate.
Four of technical scheme of the present invention realizes by following measure: a kind of preparation method who uses the polylactic acid-modified feldspar matrix material of modification feldspar, raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 5 parts to 10 parts in softening agent; The preparation method of this polylactic acid-modified feldspar matrix material carries out as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Be four further optimization and/or improvements to the foregoing invention technical scheme below:
The preparation method of the polylactic acid-modified feldspar matrix material of above-mentioned use modification feldspar, raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 0.1 part to 1 part of nucleator, 5 parts to 10 parts in softening agent; The preparation method of this polylactic acid-modified feldspar matrix material carries out as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature; Or/and nucleator is more than one mixtures in talcum powder, carbon nanotube, calcium carbonate, clay and the amides; Or/and softening agent is more than one mixtures in polyoxyethylene glycol, organic acid acetic, phosphoric acid ester, polyester and the tributyl acetylcitrate.
Five of technical scheme of the present invention realizes by following measure: the goods that a kind of polylactic acid-modified feldspar matrix material that uses the modification feldspar is produced.
The interface contact angle of the modification feldspar that the present invention obtains is big, surface hydrophilicity weakens is that surperficial lipophilicity strengthens, and makes the feldspar surface realize organic modification, can form the good interface consistency with polylactic acid based body, forms good dispersion at the interface; The polylactic acid-modified feldspar matrix material that obtains by the modification feldspar is significantly increased than mechanical property, thermostability and the toughness of poly(lactic acid) base material, thereby has expanded the Application Areas of poly(lactic acid), has great application prospect.
Description of drawings
Accompanying drawing 2 is the contact angle image of the existing wet-process modified feldspar of KH570.
Accompanying drawing 3 is the contact angle image of modification feldspar of the present invention.
Accompanying drawing 4 is the TG curve comparison diagram of existing poly(lactic acid) base material curve 1 with the polylactic acid-modified feldspar matrix material of the present invention curve 2.
Accompanying drawing 5 is the DTG curve comparison diagram of existing poly(lactic acid) base material curve 1 with the polylactic acid-modified feldspar matrix material of the present invention curve 2.
Accompanying drawing 6 is the shock resistance section SEM figure of existing poly(lactic acid) base material.
Accompanying drawing 7 is the shock resistance section SEM figure of the polylactic acid-modified feldspar matrix material of the present invention.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme of the present invention and practical situation.
Embodiment 3, as the optimization of above-described embodiment, in the first step of embodiment 3, add in the dehydrated alcohol Feldspar Powder after pulverizing and stirring, stirring velocity is that 400 rev/mins to 2000 rev/mins, churning time are 30 minutes to 60 minutes, obtains Feldspar Powder suspension after the stirring.
Embodiment 4, as the optimization of above-described embodiment, in the 3rd step of embodiment 4, modification feldspar slurry is filtered, filter cake after the filtration is 100 ℃ to 105 ℃ down after dry 2 hours to 3 hours in temperature, is ground into particle diameter and is 60 microns to 74 microns to obtain the modification feldspar.
Embodiment 5, and as the optimization of above-described embodiment, the properties-correcting agent of embodiment 5 is more than one mixtures in silane coupling agent, titanate coupling agent and the aluminate coupling agent.
Embodiment 6, and this uses the polylactic acid-modified feldspar matrix material of modification feldspar, and raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Embodiment 7, and this uses the polylactic acid-modified feldspar matrix material of modification feldspar, and raw material contains 100 parts of polylactic resin by weight, 1 part or 10 parts of modification feldspar, 5 parts or 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Embodiment 8, and this uses the polylactic acid-modified feldspar matrix material of modification feldspar, and raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 0.1 part to 1 part of nucleator, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Embodiment 9, and this uses the polylactic acid-modified feldspar matrix material of modification feldspar, and raw material contains 100 parts of polylactic resin by weight, 1 part or 10 parts of modification feldspar, 0.1 part or 1 part of nucleator, 5 parts or 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
Embodiment 10, and as the optimization of above-described embodiment, the nucleator of embodiment 10 is more than one mixtures in talcum powder, carbon nanotube, calcium carbonate, clay and the amides;
Embodiment 11, and as the optimization of above-described embodiment, the softening agent of embodiment 11 is more than one mixtures in polyoxyethylene glycol, organic acid acetic, phosphoric acid ester, polyester and the tributyl acetylcitrate.
Embodiment 12, the goods that this uses the polylactic acid-modified feldspar matrix material of modification feldspar to produce.
Be the test result to above-described embodiment gained modification feldspar and polylactic acid-modified feldspar matrix material below:
1. interface contact angle test (the interface contact angle is analyzed: in employings marine morning digital technique company limited JJ2000B2 contact angle measurement mensuration)
By measuring liquid (water droplet) at the contact angle of sample surfaces, can compare the wetting ability of sample surfaces and liquid in the wettability of sample surfaces, from the surface properties of macroscopic view reflection powder.From Fig. 1, Fig. 2 and Fig. 3 as can be seen, unmodified feldspar surface possess hydrophilic property, contact angle is 23.0 °, and the wetting ability of the modification feldspar of the wet-process modified feldspar of KH570 and gained of the present invention obviously to weaken be that lipophilicity obviously strengthens, make the feldspar surface realize organic modification, the contact angle of the modification feldspar of the wet-process modified feldspar of KH570 and gained of the present invention is respectively 120.99 °, 133.49 °; Interface contact angle test shows, the modification feldspar of the wet-process modified feldspar of KH570 and gained of the present invention is compared with unmodified feldspar, the interface contact angle of the modification feldspar of the wet-process modified feldspar of KH570 and gained of the present invention obviously increases, and the surface has lipophilicity, and considerable change has taken place surface property; The modification feldspar of gained of the present invention is compared with the wet-process modified feldspar of KH570, and the modified effect of the modification feldspar of gained of the present invention obviously is better than the wet-process modified feldspar of KH570.
2. performance test
2.1 mechanics property analysis
Goods to the polylactic acid-modified feldspar matrix material of above-described embodiment gained and production carry out performance test, tension test: adopt American I nstron 4302 type universal testing machines, test its maximum fracture tensile strength and elongation at break according to standard GB/T8804. 2-2003, shock-testing machine, XJU-22, by standard GB1843-2002, impact velocity 3.5 m/s, adopt automatic breach sampling machine to prepare v-notch, gap width 2 mm, measure breach residue width and residual thickness, test after at room temperature placing 24 h.Its concrete test result is as follows: the average mechanical property of the polylactic acid-modified feldspar matrix material of gained of the present invention and the goods of production and the average mechanics performance comparison data of poly(lactic acid) base material are as shown in table 1.
Table 1
| ? | Resistance to impact shock (KJ/m 2） | Tensile strength (MPa) | Elongation at break (%) |
| The goods of the polylactic acid-modified feldspar matrix material of the present invention and production | 3.6 to 5.9 | 49.60 to 56.59 | 8.66 to 11.22 |
| Prior art poly(lactic acid) base material | 2.9 | 48.21 | 4.74 |
As can be seen from Table 1, average mechanical property resistance to impact shock, tensile strength and the elongation at break of poly(lactic acid) base material are respectively 2.9 KJ/m
2, 48.21 MPa, 4.74%; Average mechanical property resistance to impact shock, tensile strength and the elongation at break of the polylactic acid-modified feldspar matrix material of gained of the present invention and the goods of production are respectively 3.6KJ/m
2To 5.9 KJ/m
2, 49.60MPa to 56.59MPa, 8.66% to 11.22%; The average mechanical property (resistance to impact shock, tensile strength and elongation at break) that the goods of the polylactic acid-modified feldspar matrix material of gained of the present invention and production are described is significantly increased than the average mechanical property (resistance to impact shock, tensile strength and elongation at break) of poly(lactic acid) base material, thereby expanded the Application Areas of poly(lactic acid), had great application prospect.
2.2 thermal stability analysis (TGA analysis)
Adopt U.S. TA Q600 thermogravimetric analyzer to carry out thermogravimetic analysis (TGA), thus the thermostability of analytic sample.Sample quality 5 mg to 10 mg, test condition: 10 ℃/min of temperature rise rate, test specification is 20 ℃ to 600 ℃, N
2Gas atmosphere.Have the TG curve comparison diagram of poly(lactic acid) base material and the polylactic acid-modified feldspar matrix material of the present invention now as shown in Figure 4, curve 1 is the TG curve of existing poly(lactic acid) base material in Fig. 4, and curve 2 is the TG curve of the polylactic acid-modified feldspar matrix material of the present invention in Fig. 4; The DTG curve comparison diagram of existing poly(lactic acid) base material and the polylactic acid-modified feldspar matrix material of the present invention as shown in Figure 5, curve 1 is the DTG curve of existing poly(lactic acid) base material in Fig. 5, and curve 2 is the DTG curve of the polylactic acid-modified feldspar matrix material of the present invention in Fig. 5; By Fig. 4 and Fig. 5 as can be seen, the heat decomposition temperature of the polylactic acid-modified feldspar matrix material of gained of the present invention has improved 12.33 ℃ than the heat decomposition temperature of prior art poly(lactic acid) base material, and the thermostability of the polylactic acid-modified feldspar matrix material of this explanation gained of the present invention is greatly improved than the thermostability of prior art poly(lactic acid) base material.
2.3 toughness relatively
Adopt the Dutch Inspect F of FEI Co. type scanning electronic microscope, acceleration voltage 20kV gets the batten after the shock resistance experiment thrusts, and surperficial metal spraying is observed its cross-section morphology under scanning electronic microscope then.
The shock resistance section SEM of prior art poly(lactic acid) base material schemes as shown in Figure 6, and the shock resistance section SEM of the polylactic acid-modified feldspar matrix material of gained of the present invention schemes as shown in Figure 7.As can be seen from Figure 6, prior art poly(lactic acid) base material shock resistance section surface is more smooth, presents the brittle rupture feature.As can be seen from Figures 6 and 7, the polylactic acid-modified feldspar matrix material of gained of the present invention is compared with prior art poly(lactic acid) base material, the wire drawing shape that evenly loosens and the part that has fine particle have appearred on the polylactic acid-modified feldspar matrix material of the gained of the present invention shock resistance section, have typical ductile rupture feature, the toughness that the polylactic acid-modified feldspar matrix material of gained of the present invention is described thus is significantly improved than the toughness of prior art poly(lactic acid) base material.
Above technical characterictic has constituted embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease non-essential technical characterictic according to actual needs, satisfies the demand of different situations.
Claims (9)
1. modification feldspar, it is characterized in that obtaining by following step: the first step, getting an amount of Feldspar Powder, to be broken to particle diameter be 60 microns to 74 microns Feldspar Powder, Feldspar Powder after the pulverizing adds in the dehydrated alcohol and stirs, obtain Feldspar Powder suspension after stirring, the mass percent concentration of Feldspar Powder in Feldspar Powder suspension is 5% to 30%; Second step, join 0.5 gram to 10 gram properties-correcting agent by 100 gram feldspars and take by weighing properties-correcting agent, it is to be made into the properties-correcting agent hydrolyzed solution in 50% to 90% the ethanolic soln that the properties-correcting agent that takes by weighing is dissolved in concentration of volume percent, the mass percent concentration of properties-correcting agent in the properties-correcting agent hydrolyzed solution is 16.7% to 50%, the Feldspar Powder suspension that the first step is obtained joins in the properties-correcting agent hydrolyzed solution and is stirred into mixed solution, regulate the pH value to 3.5 of mixed solution, mixed solution hydrolysis after the adjusting pH value places it in the microwave reactor after 30 minutes to 120 minutes, is that microwave exposure obtains modification feldspar slurry under 20 W to 50W after 20 minutes to 60 minutes at power; The 3rd step, modification feldspar slurry is filtered, obtain the modification feldspar after the filter cake drying after the filtration, the pulverizing.
2. modification feldspar according to claim 1, it is characterized in that in the first step, Feldspar Powder after will pulverizing adds in the dehydrated alcohol and stirs, and stirring velocity is that 400 rev/mins to 2000 rev/mins, churning time are 30 minutes to 60 minutes, obtains Feldspar Powder suspension after the stirring; Or/and, the 3rd step, modification feldspar slurry is filtered, the filter cake after the filtration is 100 ℃ to 105 ℃ down after dry 2 hours to 3 hours in temperature, is ground into particle diameter and is 60 microns to 74 microns to obtain the modification feldspar; Or/and properties-correcting agent is more than one mixtures in silane coupling agent, titanate coupling agent and the aluminate coupling agent.
3. the preparation method of a modification feldspar, it is characterized in that being undertaken by following step: the first step, getting an amount of Feldspar Powder, to be broken to particle diameter be 60 microns to 74 microns Feldspar Powder, Feldspar Powder after the pulverizing adds in the dehydrated alcohol and stirs, obtain Feldspar Powder suspension after stirring, the mass percent concentration of Feldspar Powder in Feldspar Powder suspension is 5% to 30%; Second step, join 0.5 gram to 10 gram properties-correcting agent by 100 gram feldspars and take by weighing properties-correcting agent, it is to be made into the properties-correcting agent hydrolyzed solution in 50% to 90% the ethanolic soln that the properties-correcting agent that takes by weighing is dissolved in concentration of volume percent, the mass percent concentration of properties-correcting agent in the properties-correcting agent hydrolyzed solution is 16.7% to 50%, the Feldspar Powder suspension that the first step is obtained joins in the properties-correcting agent hydrolyzed solution and is stirred into mixed solution, regulate the pH value to 3.5 of mixed solution, mixed solution hydrolysis after the adjusting pH value places it in the microwave reactor after 30 minutes to 120 minutes, is that microwave exposure obtains modification feldspar slurry under 20 W to 50W after 20 minutes to 60 minutes at power; The 3rd step, modification feldspar slurry is filtered, obtain the modification feldspar after the filter cake drying after the filtration, the pulverizing.
4. the preparation method of a modification feldspar according to claim 3, it is characterized in that in the first step, add in the dehydrated alcohol Feldspar Powder after pulverizing and stirring, stirring velocity is that 400 rev/mins to 2000 rev/mins, churning time are 30 minutes to 60 minutes, obtains Feldspar Powder suspension after the stirring; Or/and, the 3rd step, modification feldspar slurry is filtered, the filter cake after the filtration is 100 ℃ to 105 ℃ down after dry 2 hours to 3 hours in temperature, is ground into particle diameter and is 60 microns to 74 microns to obtain the modification feldspar; Or/and properties-correcting agent is more than one mixtures in silane coupling agent, titanate coupling agent and the aluminate coupling agent.
5. the polylactic acid-modified feldspar matrix material of right to use requirement 1 or 2 described modification feldspars is characterized in that raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
6. polylactic acid-modified feldspar matrix material according to claim 5 is characterized in that raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 0.1 part to 1 part of nucleator, 5 parts to 10 parts in softening agent; This polylactic acid-modified feldspar matrix material obtains as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature; Or/and nucleator is more than one mixtures in talcum powder, carbon nanotube, calcium carbonate, clay and the amides; Or/and softening agent is more than one mixtures in polyoxyethylene glycol, organic acid acetic, phosphoric acid ester, polyester and the tributyl acetylcitrate.
7. the preparation method of the polylactic acid-modified feldspar matrix material of right to use requirement 1 or 2 described modification feldspars is characterized in that raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 5 parts to 10 parts in softening agent; The preparation method of this polylactic acid-modified feldspar matrix material carries out as follows: polylactic resin, modification feldspar and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature.
8. the preparation method of polylactic acid-modified feldspar matrix material according to claim 7 is characterized in that raw material contains 100 parts of polylactic resin by weight, 1 part to 10 parts of modification feldspar, 0.1 part to 1 part of nucleator, 5 parts to 10 parts in softening agent; The preparation method of this polylactic acid-modified feldspar matrix material carries out as follows: polylactic resin, modification feldspar, nucleator and the softening agent of aequum are fully mixed through stirring mixer, and entering single screw extrusion machine then is to extrude under 170 ℃ to 190 ℃ to obtain polylactic acid-modified feldspar matrix material at extrusion temperature; Or/and nucleator is more than one mixtures in talcum powder, carbon nanotube, calcium carbonate, clay and the amides; Or/and softening agent is more than one mixtures in polyoxyethylene glycol, organic acid acetic, phosphoric acid ester, polyester and the tributyl acetylcitrate.
9. a right to use requires the goods that 5 or 6 described polylactic acid-modified feldspar matrix materials are produced.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754309A (en) * | 2016-03-24 | 2016-07-13 | 湖州新奥克化工有限公司 | Preparation method of PHA (polyhydroxyalkanoate)-based composite |
| CN106518148A (en) * | 2016-11-11 | 2017-03-22 | 中石化节能环保工程科技有限公司 | Ceramsite with lipophilic characteristic and preparation method of ceramsite |
| CN106518147A (en) * | 2016-11-11 | 2017-03-22 | 中石化节能环保工程科技有限公司 | Oleophylic ceramsite adopting oil-based drilling cutting residues obtained after thermal decomposition and preparation method of oleophylic ceramsite |
| CN106747371A (en) * | 2016-11-11 | 2017-05-31 | 中石化节能环保工程科技有限公司 | Ceramic fracturing sand with oil-wet behavior and preparation method thereof |
| CN111647287A (en) * | 2020-06-12 | 2020-09-11 | 广西夏阳环保科技有限公司 | Surface modification method of kaolin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101235194A (en) * | 2008-03-03 | 2008-08-06 | 新疆大学 | Polylactic acid-modified grammite composite material and preparation method thereof |
| CN101801636A (en) * | 2007-09-12 | 2010-08-11 | 花王株式会社 | Process for production of injection-molded article of polylactic acid resin |
-
2013
- 2013-04-22 CN CN201310143173.4A patent/CN103275473B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101801636A (en) * | 2007-09-12 | 2010-08-11 | 花王株式会社 | Process for production of injection-molded article of polylactic acid resin |
| CN101235194A (en) * | 2008-03-03 | 2008-08-06 | 新疆大学 | Polylactic acid-modified grammite composite material and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754309A (en) * | 2016-03-24 | 2016-07-13 | 湖州新奥克化工有限公司 | Preparation method of PHA (polyhydroxyalkanoate)-based composite |
| CN106518148A (en) * | 2016-11-11 | 2017-03-22 | 中石化节能环保工程科技有限公司 | Ceramsite with lipophilic characteristic and preparation method of ceramsite |
| CN106518147A (en) * | 2016-11-11 | 2017-03-22 | 中石化节能环保工程科技有限公司 | Oleophylic ceramsite adopting oil-based drilling cutting residues obtained after thermal decomposition and preparation method of oleophylic ceramsite |
| CN106747371A (en) * | 2016-11-11 | 2017-05-31 | 中石化节能环保工程科技有限公司 | Ceramic fracturing sand with oil-wet behavior and preparation method thereof |
| CN111647287A (en) * | 2020-06-12 | 2020-09-11 | 广西夏阳环保科技有限公司 | Surface modification method of kaolin |
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