Process for treatment of nanoparticles of mineral filler for use in polymerization in the presence of nanoparticles

Patent metadata

Field	Value
Publication number	US-2018002529-A1
Application number	US-201415540513-A
Country	US
Kind code	A1
Filing date	Dec 29, 2014
Priority date	Dec 29, 2014
Publication date	Jan 4, 2018
Grant date	—

Abstract

A process for treatment of nanoparticles of mineral filler for obtaining 5 processed nanoparticles for use in polymerization in the presence of nanopartciles which includes the steps of (a) drying a mineral filler with an inert gas for remove catalyst poisons; (b) mixing the mineral filler dried obtained in step (a) with a swelling agent in a liquid state or near a critical state or in the supercritical state; (c) subjecting the swelling agent of the 10 mixture obtained in step (b) to an endoenthalpic or isoentalphic phase change by altering the conditions of the temperature and/or pressure; (d) subjecting the nanoparticles of the mixture obtained in step (c) to contact of scavenging agent to react with catalyst poisons; then the mixture obtained in step (d) can be dried in a step (e) with an inert gas to remove sub-products 15 from scavenging agent and catalyst poisons to obtain the treated nanoparticles.

First claim

What is claimed is:

1 . A process for treatment of nanoparticles of a mineral filler, which comprises the steps of:
a. Drying a mineral filler with an inert gas; b. Mixing the dried mineral filler obtained in step (a) with a swelling agent in a liquid state, or near a critical state or in a supercritical state; c. Subjecting the swelling agent of the mixture obtained in step (b) to an endoenthalpic or isoenthalpic phase change, by altering the conditions of temperature and/or pressure; and d. Subjecting the mixture obtained in step (c) to contact with a scavenging agent.

2 . The process as claimed in claim wherein step (a) occurs in a temperature range of 20 to 160° C., preferably between 100 and 120° C., at a pressure range of from 0 to 16.000 mmHga, preferably between 0 and 740 mmHga, for a period of time varying between 2 and 24 hours, preferably from 4 to 8 hours

3 . The process as claimed in claim wherein step (a) occurs using a dynamic drying system selected from the group consisting of a fluidized bed dryer, a rotary dryer and a rolling bed dryer.

4 . The process as claimed in claim 1 , wherein step (b) occurs in a continuous or batch process.

5 . The process as claimed in claim 1 , wherein step (b) is conducted in a stirred reactor.

6 . The process as claimed in claim 1 , wherein the step (b) duration varies between 1 and 10 hours, preferably between 2 and 6 hours.

7 . The process as claimed in claim 1 , wherein step (c) occurs in the presence of a scavenging agent.

8 . The process as claimed in claim 1 , wherein in step (c) the endoenthalpic or isoenthalpic phase change occurs by transferring the mixture containing the mineral filler and the swelling agent to a second reactor.

9 . The process as claimed in claim 8 , wherein the second reactor is selected from the group consisting of a CSTR type reactor, a continuous or batch stirred flow reactor and a fluidized bed reactor.

10 . The process as claimed in claim 1 , wherein step (d) occurs in a polymerization reactor.

11 . The process as claimed in claim 1 , wherein in step (d) the time of contact of the mineral filler with the scavenging agent varies from 0.1 to 600 minutes, preferably between 30 to 120 minutes.

12 . The process as claimed in claim 1 , wherein the mineral filler obtained in step (d) is, optionally, dried with an inert gas in a step (e).

13 . The process as claimed in claim 12 , wherein step (e) is carried out using the same inert gas and same conditions used in step (a).

14 . The process as claimed in claim 1 , wherein the mineral filler is a sheet-like (layered) filler or spherical-like filler.

15 . The process as claimed in claim 15 , wherein the spherical-like mineral filler is selected from the group consisting of ZnO, CdO, Ca 2 O, TiO 2 , Al 2 O 3 , SiO 2 , Fe 3 O 4 , CaCO 3 and silver particles.

16 . The process as claimed in claim 15 , wherein the sheet-like mineral filler is selected from the group consisting of hydrophilic or organophilic natural or synthetic phyllosilicates, micas, kaolinites and graphite.

17 . The process as claimed in claim 1 , wherein the mineral filler is graphene.

18 . The process as claimed in claim 1 , wherein the mineral filler is a carbon nanotube.

19 . The process as claimed in claim 1 , wherein the inert gas is nitrogen or a saturated hydrocarbon.

20 . The process as claimed in claim 19 , wherein the saturated hydrocarbon is methane, ethane, propane or butane.

21 . The process as claimed in claim 1 , wherein the swelling agent is a saturated or unsaturated hydrocarbon.

22 . The process as claimed in claim 21 , wherein the swelling agent is selected from the group consisting of ethane, propane, butane, pentane, hexane, heptanes, octane, propylene, 1-butene, 1-pentene, 1-hexene and 1-octene.

23 . The process as claimed in claim 1 , wherein the swelling agent is added in an amount of 50 to 1000% by weight based on the weight of the mineral filler, preferably 50 to 200% by weight based on the weight of the mineral filler.

24 . The process as claimed in claim 1 , wherein the scavenging agent is a metallic hydride or an organometallic compound.

25 . The process as claimed in claim 24 , wherein the scavenging agent is an alkylaluminium or an alkylaluminoxane.

26 . The process as claimed in claim 24 , wherein the scavenging agent has the general formula I, II, III, IV, V or VI:

Wherein:
M 1 is Al or B;
M 2 is Zn or Mg;
R is a hydrocarbyl group between 1 to 8 carbons or hydrogen; and
X is Cl, I or O.

27 . The process as claimed in claim 1 , wherein the scavenging agent is added in an amount of 1 to 50% by weight based on the weight of the mineral filler, preferably in an amount of 1 to 20% by weight based on the weight of the mineral filler.

28 . Nanoparticles treated by the process as claimed in claim 1 .

29 . Use of nanoparticles according to claim 28 to produce nanocomposites.

30 . Use of nanoparticles according to claim 29 to produce polyolefin nanocomposites.

Assignees

• Braskem Sa

Inventors

• Pozzer Dihogenes Adriano
• Junior Olavo Martins
• Lucas Alessandra Coelho Silva
• Silveira Fernando

Classifications

• Y10S977/734

  Fullerenes, i.e. graphene-based structures, such as nanohorns, nanococoons, nanoscrolls or fullerene-like structures, e.g. WS2 or MoS2 chalcogenide nanotubes, planar C3N4, etc. · CPC title

• Y10S977/742

  Carbon nanotubes, CNTs · CPC title

• Y10S977/90

  having step or means utilizing mechanical or thermal property, e.g. pressure, heat · CPC title

• Y10S977/845

  Purification or separation of fullerenes or nanotubes · CPC title

• Y10S977/811

  Of specified metal oxide composition, e.g. conducting or semiconducting compositions such as ITO, ZnOx · CPC title