CN1341677A - Method for preparing polymer ultra-fine micropowder by means of grinding block force chemical reactor - Google Patents

Method for preparing polymer ultra-fine micropowder by means of grinding block force chemical reactor Download PDF

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Publication number
CN1341677A
CN1341677A CN 00113155 CN00113155A CN1341677A CN 1341677 A CN1341677 A CN 1341677A CN 00113155 CN00113155 CN 00113155 CN 00113155 A CN00113155 A CN 00113155A CN 1341677 A CN1341677 A CN 1341677A
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polymkeric substance
chemical reactor
ultra
fine micropowder
pan type
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CN 00113155
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CN1172978C (en
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王琪
陈哲
刘长生
夏和生
卢灿辉
徐僖
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Sichuan University
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Sichuan University
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Abstract

The method for preparing polymer superfine micropowder by using grinding block mechanochemical reactor is characterized by that it utilizes the strong extrusion shearing force produced by unique structure of Chinese patent (ZL95 2 42817.2) grinding block mechanochemical reactor or under the common action of optimum grinding adjuvant to implement pulverization and ultramicro refinement. The grain size of said invented superfine micropowder is 30nm-50 micrometers. It can be extensively used in the fields of paint, adhesive, ink, solid lubricant, cosmetics and biomedicine material. Said invention features of solid phase pulverization, room temp., simple and convenient, without need of acid or alkali medium, saving energy, no environmental pollution and easy to implement commercial production.

Description

Pan type physico chemical reactor prepares the method for polymkeric substance ultra-fine micropowder
The present invention relates to a kind of method for preparing the polymkeric substance ultra-fine micropowder.
The polymkeric substance ultra-fine micropowder is the polymer powder materials that micron arrives nano-scale that has through certain technological process preparation.Have particular performances, can be widely used in fields such as coating, tackiness agent, solid lubricant, ink, makeup and biomedical material, be subjected to various countries scholar's great attention in recent years, become one of the research focus in material field.But because toughness of polymers is big, softening temperature is low, the ultra micro refinement has suitable difficulty.For addressing this problem, people mainly adopt following several method: (1) solution deposit; (2) emulsion method; (3) direct polymerization method; (4) mechanical crushing method (deep cooling comminuting method, section method and comminution by gas stream).Wherein mechanical crushing method technology is simple, the large-scale continuous industrial production of energy, and yield height, but energy consumption height need deep cooling to pulverize to the obdurability polymkeric substance, need use acid-alkali medium sometimes, and be difficult for reaching very small particle size.
The method that provides a kind of pan type physico chemical reactor to prepare the polymkeric substance ultra-fine micropowder at the deficiencies in the prior art is provided, is characterized in that pan type physico chemical reactor is introduced ultrafine powder prepares frontier.Utilize the present inventor to obtain the powerful extrusion shearing power that Patent right pan type physico chemical reactor unique texture produces, or under preferred grinding aid acting in conjunction, realize polymkeric substance pulverizing and ultra micro refinement.The ultra-fine micropowder granularity that makes is 30nm-50 μ m.
Purpose of the present invention is realized by following technical measures.
Pan type physico chemical reactor prepares the method for polymkeric substance ultra-fine micropowder:
1. with particle diameter independent or several mixture of polymers of granular or powdery polymer or the polymerization of 0.5-5mm
Thing and grinding aid uniform mixing add pan type physico chemical reactor, and it is back along the discharging of mill edge to mill,
Finish once and mill, milling through 5-55 circulation to make 30nm-50 μ m polymkeric substance ultra-fine micropowder.
2. the condition of milling: envrionment temperature is 0-40 ℃,
The recirculated cooling water temperature is 1-40 ℃,
Speed of grinding plate is 15-100rpm,
The cycle index of milling is 5-55 time.
The polymkeric substance initial particle is 0.5-5mm, and polymkeric substance is commodity polymer such as polyethylene, polypropylene, polystyrene, polyvinyl chloride; Engineering plastics such as polymeric amide (PA-6, PA-66, PA-610, PA-1010), polyester, polyethers, polyimide; The multipolymer of elastomerics such as natural rubber, styrene-butadiene rubber(SBR), paracril, chloroprene rubber, SBS thermoplastic elastomer, polyurethane termoplastic elastomer and above-mentioned polymer monomer.
Grinding aid comprises metal oxide such as SiO 2, TiO 2, Al 2O 3Metal-powder such as iron powder, copper powder, zinc powder; Inorganic salt such as BaSO 4, CaCO 3Natural mineral such as water-ground limestone, wollastonite, kaolin, polynite, quartz, mica, graphite and/or positively charged ion, negatively charged ion or nonionic organic surface active agent.
Can prepare the single polymers ultra-fine micropowder, also can prepare the mixed polymer ultra-fine micropowder, can also prepare the blend polymer ultra-fine micropowder, also can prepare inorganics/polymkeric substance composite superfine micro mist.
The product of the present invention's preparation is the polymkeric substance ultra-fine micropowder of 30nm-50 μ m size.Can be widely used in fields such as coating, tackiness agent, ink, solid lubricant, makeup and biomedical material.
The present invention has following characteristics:
(1) pan type physico chemical reactor is patented product (ZL95242817.2), and equipment is simple, and is easy to operate;
(2) room temperature is pulverized;
(3) wide to the polymkeric substance suitability;
(4) the product granularity scope is adjustable, controlled.
Embodiment:
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
1. check that pan type physico chemical reactor is in shape, at ambient temperature, connect water coolant, startup is established
Be equipped with, the adjustment rotating speed is 30rpm, adds particle diameter 3-5mm polypropylene particles from opening for feed, after milling, and the edge
The discharging of mill edge is finished once and is milled.Circulation is milled 14 times continuously, and can make median size is 35-50 μ m
The polypropylene powder.
2. at ambient temperature, connect water coolant, starting outfit, adjusting rotating speed is 35 commentaries on classics, adds from opening for feed simultaneously
Particle diameter 3-5mm PA-6 particle and particle diameter 10 μ wollastonite grinding aids, after milling, along the discharging of mill edge,
Finish once and mill.Circulation is milled 28 times continuously, can get median size to be after separating the removal grinding aid
The PA-6 powder of 30-80nm.
3. at ambient temperature, connect water coolant, starting outfit, adjusting rotating speed is 55 commentaries on classics, adds through ten from opening for feed
The particle diameter 3-5mm polystyrene particle that six alkyl trimethyl ammonium bromides are handled is after milling, along the mill edge
Discharging is finished once and is milled.Circulation is milled 18 times continuously, can get median size after separating the removal grinding aid
Polystyrene powder for 150-200nm.

Claims (3)

1. pan type physico chemical reactor prepares the method for polymkeric substance ultra-fine micropowder, it is characterized in that:
(1) with independent or several mixture of polymers of the granular or powdery polymer of particle diameter 0.5-5mm or polymkeric substance
With the grinding aid uniform mixing, add pan type physico chemical reactor, it is back along the discharging of mill edge to mill,
Finish once and mill, milling through 5-55 circulation to make 30nm-50 μ m polymkeric substance ultra-fine micropowder,
(2) condition of milling: envrionment temperature is 0-40 ℃,
The recirculated cooling water temperature is 1-40 ℃,
Speed of grinding plate is 15-100rpm,
The cycle index of milling is 5-55 time.
2. the method for preparing the polymkeric substance ultra-fine micropowder according to the described pan type physico chemical reactor of claim 1 is characterized in that polymkeric substance is that polyethylene, polypropylene, polystyrene, polyvinyl chloride, polymeric amide, polyester, polyethers, polyimide, natural rubber, styrene-butadiene rubber(SBR), paracril, chloroprene rubber, SBS thermoplastic elastomer, polyurethane termoplastic elastomer are at least a.
3. the method for preparing the polymkeric substance ultrafine powder according to the described pan type physico chemical reactor of claim 1. is characterized in that grinding aid is SiO 2, TiO 2, A1 2O 3, iron powder, copper powder, zinc powder, BaSO 4, CaCO 3, water-ground limestone, wollastonite, kaolin, polynite, quartz, mica, graphite or positively charged ion, negatively charged ion or nonionic organic surface active agent be at least a.
CNB001131559A 2000-09-04 2000-09-04 Method for preparing polymer ultra-fine micropowder by means of grinding block force chemical reactor Expired - Lifetime CN1172978C (en)

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CNB001131559A CN1172978C (en) 2000-09-04 2000-09-04 Method for preparing polymer ultra-fine micropowder by means of grinding block force chemical reactor

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CN1341677A true CN1341677A (en) 2002-03-27
CN1172978C CN1172978C (en) 2004-10-27

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008131643A1 (en) * 2007-04-25 2008-11-06 Huihong Chen Method and apparatus for combined recycling of waste polymer material or joint production with carbon black
CN100509881C (en) * 2006-09-11 2009-07-08 四川大学 Method for improving processing capability of metallocene polyethylene
CN102420318A (en) * 2011-12-02 2012-04-18 华南理工大学 Preparing method of alumina-carbon base composite material for negative electrode of lithium ion battery
CN101402745B (en) * 2007-04-25 2012-07-04 陈汇宏 Method and apparatus for combination regeneration, or coproduction with hydrocarbon black of waste and old macromolecule material
CN104327374A (en) * 2014-10-08 2015-02-04 四川大学 Waste circuit board non-metal ultra-fine powder, waste circuit board non-metal ultra-fine powder and polyolefin composite material, and preparation methods of the powder and the composite material
CN111036342A (en) * 2019-12-05 2020-04-21 四川大学 Preparation device and preparation process of polymer-based spherical powder
CN111533978A (en) * 2020-05-26 2020-08-14 四川大学 High-value composite material for automobile broken residues and preparation method thereof
CN111873283A (en) * 2020-06-12 2020-11-03 成都普美怡科技有限公司 Method for preparing high-thermal-conductivity polymer-based product by using solid-phase shearing and grinding technology
CN115353776A (en) * 2022-08-16 2022-11-18 四川大学 Waste polypropylene-based super-hydrophobic coating and preparation method thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100509881C (en) * 2006-09-11 2009-07-08 四川大学 Method for improving processing capability of metallocene polyethylene
WO2008131643A1 (en) * 2007-04-25 2008-11-06 Huihong Chen Method and apparatus for combined recycling of waste polymer material or joint production with carbon black
CN101402745B (en) * 2007-04-25 2012-07-04 陈汇宏 Method and apparatus for combination regeneration, or coproduction with hydrocarbon black of waste and old macromolecule material
CN102420318A (en) * 2011-12-02 2012-04-18 华南理工大学 Preparing method of alumina-carbon base composite material for negative electrode of lithium ion battery
CN104327374A (en) * 2014-10-08 2015-02-04 四川大学 Waste circuit board non-metal ultra-fine powder, waste circuit board non-metal ultra-fine powder and polyolefin composite material, and preparation methods of the powder and the composite material
CN111036342A (en) * 2019-12-05 2020-04-21 四川大学 Preparation device and preparation process of polymer-based spherical powder
CN111533978A (en) * 2020-05-26 2020-08-14 四川大学 High-value composite material for automobile broken residues and preparation method thereof
CN111873283A (en) * 2020-06-12 2020-11-03 成都普美怡科技有限公司 Method for preparing high-thermal-conductivity polymer-based product by using solid-phase shearing and grinding technology
CN111873283B (en) * 2020-06-12 2022-03-01 成都普美怡科技有限公司 Method for preparing high-thermal-conductivity polymer-based product by using solid-phase shearing and grinding technology
CN115353776A (en) * 2022-08-16 2022-11-18 四川大学 Waste polypropylene-based super-hydrophobic coating and preparation method thereof
CN115353776B (en) * 2022-08-16 2023-03-07 四川大学 Waste polypropylene-based super-hydrophobic coating and preparation method thereof

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