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WO2025081251A1 - Mousse polymère conductrice pour applications antistatiques et procédé de production de celle-ci - Google Patents

Mousse polymère conductrice pour applications antistatiques et procédé de production de celle-ci Download PDF

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Publication number
WO2025081251A1
WO2025081251A1 PCT/BR2024/050473 BR2024050473W WO2025081251A1 WO 2025081251 A1 WO2025081251 A1 WO 2025081251A1 BR 2024050473 W BR2024050473 W BR 2024050473W WO 2025081251 A1 WO2025081251 A1 WO 2025081251A1
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WO
WIPO (PCT)
Prior art keywords
foam
cationic cellulose
conductive agent
cellulose
foams
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/BR2024/050473
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English (en)
Portuguese (pt)
Inventor
Gabriele POLEZI
Diego Magalhaes DO NASCIMENTO
Elisa Silva FERREIRA
Juliana Da Silva BERNARDES
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Centro Nacional de Pesquisa em Energia e Materiais CNPEM
Original Assignee
Centro Nacional de Pesquisa em Energia e Materiais CNPEM
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from BR102023021652-8A external-priority patent/BR102023021652A2/pt
Application filed by Centro Nacional de Pesquisa em Energia e Materiais CNPEM filed Critical Centro Nacional de Pesquisa em Energia e Materiais CNPEM
Publication of WO2025081251A1 publication Critical patent/WO2025081251A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
    • C08B15/08—Fractionation of cellulose, e.g. separation of cellulose crystallites
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/22—After-treatment of expandable particles; Forming foamed products
    • C08J9/228—Forming foamed products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/35—Composite foams, i.e. continuous macromolecular foams containing discontinuous cellular particles or fragments

Definitions

  • the present invention relates to a conductive polymeric foam capable of being used in packaging of electrical components sensitive to electrostatic discharge.
  • the present invention falls within the field of materials chemistry.
  • Static electricity is a phenomenon that occurs when electrons flow between two different bodies when they are touched. During this process, electrons leave the surface of one object and attach themselves to the surface of the other, so that each object, after contact/separation, begins to present excess positive or negative charges.
  • ESD electrostatic discharge
  • Patent document CN106633791 A deals with a conductive film based on nanocellulose and graphene, whose alloy is made by means of synthetic latexes.
  • a cellulose composite with ferric oxide (CN 106243392), a conductive coating for paper (CN111809447B B), conductive papers (CN107700262B B, WO2011140971 A1), and an antistatic tape based on oxidized cellulose (CN116556112) are also disclosed. None of these, however, is capable of providing extra protection against mechanical shocks, in addition to performing as an anti-electrostatic discharge shield, or mentions flame retardant properties, which brings greater safety to the use of the packaging.
  • Document US20040146690 A1 concerns cardboard in which the outer paper contains poly(diallyldimethylammonium chloride), polyethylene glycol, diethanol amide or mixtures thereof, and the folded layer between the outer papers is electrically conductive and is made of carbon black. Foams, however, have the advantage of being less dense than cardboard, which facilitates the transportation and handling of the packaged material.
  • the present invention relates to a polymeric conductive foam for antistatic applications formed by cationic cellulose and a conductive agent.
  • the foam of the present invention has the advantage of using an abundant biopolymer, of renewable origin, being capable of absorbing energy values greater than 70 Jm -3 and presenting resistivities around 10 7 to 10 2 Q.cm.
  • the foam of the present invention extinguishes fire in times shorter than those required for foams currently available on the market.
  • the foam of the present invention is produced by a simple, few-step process, which comprises: a) dispersing the conductive agent in an aqueous medium containing cationic cellulose fibers, b) freezing the dispersion and c) lyophilizing the dispersion.
  • the cationized cellulose fibers allow the conductive agent to remain homogeneously dispersed in an aqueous medium, so that the freeze-drying step promotes the formation of a foam with uniform morphology, mechanical and electrical properties suitable for the proposed use.
  • Figure 1 is a photograph of carbon black dispersions in (a) water, (b) bleached cellulose, (c) cationic cellulose according to the present invention, being (i) immediately after mixing and (ii) after one week of standing.
  • FIG. 2 is a photograph of the foams of the present invention with different contents of carbon black (CB) as a conductive agent.
  • the contents are 0 (CB00), 1 (CB01), 5 (CB05), 10 (CB10), 20 (CB20) and 30% (CB30) relative to the dry mass of cationic cellulose.
  • Figure 3 shows electron microscopy images of foams (a) and (b) CB00, (c) and (d) CB01, (e) and (f) CB10, (g) and (h) CB20, (i) and (j) CB30. Scale bars of 300 pm on the left and 3 pm on the right.
  • Figure 4 shows graphs of (a) apparent density and (b) porosity of the foams of the present invention with different CB contents. Data are presented as mean ⁇ standard deviation. Different letters indicate statistically significant difference between samples (p ⁇ 0.05).
  • Figure 5 shows stress vs. strain curves of the foams of the present invention with different CB contents.
  • Figure 6 shows the compression and specific moduli (a), and stresses at 50% deformation and energies absorbed during compression of the foams of the present invention with different CB contents (b).
  • the data are presented as mean ⁇ standard deviation. Different letters in the same property indicate statistically significant difference between the samples (p ⁇ 0.05).
  • Figure 8 shows the results of the LED test, demonstrating the electrical conductivity of the foams of the present invention with different concentrations of CB.
  • Figure 9 shows photographs of the flammability test of foams (a) commercial, (b) cationic cellulose without addition of CB, (c) foam of the present invention with 5% CB and (d) with 20% CB.
  • the present invention relates to a polymeric conductive foam formed by cationic cellulose and a conductive agent.
  • the cellulose comes from sugarcane bagasse.
  • the cellulose is isolated by means of chemical pretreatments, preferably by means of an organosolve pulping process, already known in the state of the art.
  • the cellulose pulp obtained in the pretreatment step is, additionally, bleached by processes also already known in the state of the art.
  • the cationic cellulose that makes up the foam of the present invention can be produced by means of cationization processes known in the state of the art.
  • One way of obtaining cationic cellulose is described in ZAMAN, M. et al. Synthesis and characterization of cationically modified nanocrystalline cellulose.
  • the concentration of cationic cellulose in the precursor aqueous dispersion of the present invention is 1 to 4% (w/w)
  • the conductive agent can be chosen from the group comprising carbon black, graphite, carbon nanotubes and metal oxides, being, preferably carbon black, which is advantageous due to its low cost.
  • the concentration of carbon black in the foam is preferably 1 to 40% (w/w) in relation to the cationic cellulose. In a preferred embodiment, the concentration of carbon black is 10 to 30%.
  • the foam of the present invention presents three-dimensional pores with irregular arrangements and roughness due to the adsorption of aggregates of the conductive agent.
  • the apparent density of the foam is 45.0 to 55.0 mg. cm -3 and the porosity has values between 91 and 97 %.
  • the specific compression modulus of the foam can vary between 20 and 25 MPa.cm 3 .g -1 , and the energy absorbed by the foam is greater than 70 J.rrr 3 .
  • the foam of the present invention has conductive characteristics, with electrical resistivities between 107 and 102 Q.cm, values sufficient for application in antistatic packaging.
  • the fire extinguishing time of the foam of this invention is of the order of 8 to 15 s, without the need for the addition of other flame retardant agents.
  • the foam production process covered by this invention comprises the following steps: a) dispersing the conductive agent in an aqueous medium containing cationic cellulose fibers, b) freezing the dispersion and c) lyophilizing the dispersion.
  • step a) it is preferable that the cationic cellulose is in the concentration range of 1 to 4% in water.
  • the conductive agent must be slowly added to the cationic cellulose suspension under stirring, and the mixture must be homogenized with the aid of torque of 9,000 to 11,000 rpm, for 10 to 20 minutes, at a temperature of around 10 °C.
  • the mixture obtained must be added to molds and frozen in step b) for lyophilization in step c).
  • the pulp was then transferred to woven fabric bags, washed with tap water until reaching a pH close to 7, pressed manually and excess water was removed using a conventional centrifuge.
  • the solids content of the organosolve pulp was determined by a moisture balance and the material was stored in a refrigerator at 4 °C until the next step.
  • the suspension was then dialyzed for ten days with a cellulose dialysis membrane (MWCO of 22 kDa) against Milli-Q water to remove residues of any reagents and by-products.
  • MWCO cellulose dialysis membrane
  • Milli-Q water Milli-Q water
  • the prepared cationic cellulose was concentrated to 3.50% (w/w) using a vacuum drying oven at a temperature of 70 °C and a pressure of 600 mmHg.
  • Carbon black (CB) powder was slowly added to the cationic cellulose suspension, under magnetic stirring, so that all the material was incorporated into the bulk of the mixture.
  • the dispersion was homogenized using an ultra-turrax (IKA, T25) at 10,000 rpm for 15 minutes in an ice bath.
  • the frozen samples were lyophilized for 48 hours in a lyophilizer with a condenser temperature below -40 °C and a vacuum of 10 mBar to remove water by sublimation.
  • the morphology of the foams was studied using an electron microscope equipped with an ETD detector, in secondary electron mode, operating at an accelerating voltage of 5 kV.
  • the foams were cut in liquid nitrogen with the aid of a blade and the central region of each one was separated for analysis. Then, a carbon film with a thickness of approximately 5 nm was deposited on the samples using a coating equipment in the carbon wire evaporation method.
  • the apparent density (pa, mg. cm -3 ) of each foam was calculated by dividing the mass by the volume of each individual sample (Equation 4). The dimensions and mass of each foam were measured using a digital caliper (with an accuracy of 0.01 mm) and an analytical balance.
  • Pceiuiose and pCB were fixed at 1600 mg. cm -3 and 264 mg. cm -3 , respectively (Chen et al., 2019; Cabot Corporation, 2023).
  • the foams were conditioned at room temperature (20 ⁇ 2°C) and relative humidity of 21 ⁇ 5% for at least 24 hours prior to testing.
  • the uniaxial compression test was performed in a universal testing machine coupled to a 50 N load cell at a constant deformation rate of 2 mm. min -1 .
  • the compression modulus was calculated from the initial linear region (between 2 and 5% deformation) of the stress-strain curves.
  • the stress at 50% was taken as the stress value required to deform the material by 50% of its length.
  • the energy absorbed by the foam during compression was obtained by the area below the stress-strain curve between 0% and 70% deformation. Eight specimens of each sample were tested and the results are reported as mean values with standard deviation.
  • Aqueous dispersions of cationic cellulose (3.5% w/w) and CB (1%, 5%, 10%, 20% and 30% w/w with respect to cellulose content) were prepared by homogenizing the two materials in an ultra-turrax. The high shear of the agitation promoted the disaggregation of the CB nanoparticles, resulting in visually homogeneous and stable dispersions. The dispersions were transferred to cylindrical polypropylene molds, frozen in a domestic refrigerator and, finally, lyophilized to remove ice crystals. A control sample containing only cationic cellulose was also produced for comparison purposes. In general, the materials presented good structural integrity after the lyophilization process, with a regular cylindrical shape and dimensions similar to the molds used to form them. Furthermore, no detachment of carbon nanoparticles from the foam structure is observed due to the good interfacial interactions between cationic cellulose and CB.
  • Foams prepared with 1% and 5% (w/w) of CB presented specific compression moduli statistically equal to the control foam (approximately 11 MPa.cm 3 .g -1 ). This shows us that at these low CB concentrations, the carbon nanomaterial is not capable of promoting mechanical reinforcement to the foam since the formation of an interconnected network is not observed, as seen in the electron microscopy images. On the other hand, with the increase in the CB content to 10% (w/w), the value of the specific compression modulus increased by 67%, reaching 20 ⁇ 2 MPa.cm 3 .g -1 .
  • Tenacity is an important parameter to be analyzed to evaluate the mechanical performance of materials used as packaging. protective. This parameter is related to the ability of a material to absorb energy and permanently deform without fracturing.
  • the CB01 and CB05 foams presented absorbed energy values close to the control foam (between 48 and 54 J.rrr 3 ), being considered equal for a statistical analysis with p ⁇ 0.05. With the increase in the CB fraction from 5% to 10% (m/m), an increase of approximately 39% was observed in the energy absorbed by the material, reaching 75 J.rrr 3 . For foams with CB contents of 20% and 30% (m/m), the values were 80 ⁇ 8 and 88 ⁇ 12 J.rrr 3 , respectively, which are statistically equal.
  • Another parameter to describe the mechanical behavior of materials is the stress required to cause 50% deformation.
  • Foams CB00, CB01 and CB05 presented statistically equal stress at 50%, with values close to 0.085 MPa.
  • the values were 0.126 ⁇ 0.009 and 0.135 ⁇ 0.013 MPa, which do not present a statistically significant difference for p ⁇ 0.05.
  • the stress required was 0.145 ⁇ 0.021 MPa.
  • CB can act as a reinforcing agent in foams at concentrations above 10% (w/w).
  • concentrations above 10% w/w.
  • the carbon nanoparticles adhere to the cellulose surface and, above this concentration, form an interconnected network.
  • This CB layer formed causes the pore walls to become thicker and, consequently, can withstand greater mechanical stresses during the compression test.
  • the foam containing only cellulose presented insulating characteristics, with an electrical resistance value greater than the highest range of the instrument used for measurement, that is, >4.0x10 7 Q.
  • the hybrid foams with 1% and 5% (m/m) of CB had resistivity values in the order of 10 7 Q.cm, while the foam with 10% (m/m) presented resistivity equal to (1.6 ⁇ 0.1) x10 4 Q.cm, with the three compositions in the range of static-dissipative materials, according to the international standards JESD625-B and ANSI/ESD S541-2019.
  • the foams with 20% and 30% (m/m) of CB have conductive characteristics, with electrical resistivity values equal to (1.01 ⁇ 0.08) x10 3 Q.cm, and (4.0 ⁇ 0.8) x10 2 Q.cm, respectively.
  • Calculating the inverse of the resistivity of each foam we obtain its electrical conductivity. It is observed that the conductivity of the foams with ⁇ 5% (m/m) of CB is almost constant and possibly close to the conductivity of the foam containing only cellulose. At low levels of conductive particles, these are considered isolated charges, which implies that the conductivity of the hybrid material is close to the conductivity of the matrix.
  • foams with BC concentrations between 5% and 10% (m/m) we have a significant increase of three orders of magnitude in conductivity.
  • the increase in the content of conductive particles leads to a percolated state, in which the particles are not completely in direct physical contact but a conductive network is created that allows electrical transport through quantum mechanical tunneling and electron hopping through the interface formed between the particle and the polymer.
  • the BC concentration increases from 10% to 20% (m/m) and from 20% to 30% (m/m)
  • we have a moderate increase in conductivity about one order of magnitude in each range.
  • the conductive particles are already in physical contact with each other, forming an interconnected three-dimensional conductive network that promotes a continuous path for the passage of electrons.
  • the additional increase in the CB content in the hybrid foams should not significantly alter the conductivity of the material.
  • the microscopy images obtained for each foam with different CB concentrations corroborate the visualization of the conductive network formed by the connected particles.
  • the percolation threshold of the system is between 5% and 10% (w/w) of CB.
  • the percolation theory is applied. These data can be obtained experimentally from the linear fit of the data to a log(o) curve as a function of log( ⁇ pf — cpc), as shown in the graph inserted in Figure 7b.
  • the best-fitting data to the percolation theory model were achieved with values of 8.0% (m/m) of CB and 1.54 for ⁇ p c et, respectively.

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  • Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Analytical Chemistry (AREA)
  • Composite Materials (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

La présente invention concerne une mousse polymère conductrice formée par une cellulose fonctionnalisée et un agent conducteur, ainsi que son procédé de production. La mousse peut être utilisée dans des emballages antistatiques et possède un pouvoir ignifuge supérieur à celui des mousses disponibles pour ce type d'application.
PCT/BR2024/050473 2023-10-18 2024-10-17 Mousse polymère conductrice pour applications antistatiques et procédé de production de celle-ci Pending WO2025081251A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BR1020230216528 2023-10-18
BR102023021652-8A BR102023021652A2 (pt) 2023-10-18 Espuma polimérica condutora para aplicações antiestáticas e processo de produção da mesma

Publications (1)

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WO2025081251A1 true WO2025081251A1 (fr) 2025-04-24

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992006239A1 (fr) * 1990-10-09 1992-04-16 Instytut Wlokiennictwa Ameliorations concernant les fibres conductrices
US8012550B2 (en) * 2006-10-04 2011-09-06 3M Innovative Properties Company Ink receptive article
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US10109386B2 (en) * 2013-05-17 2018-10-23 Heraeus Medical Components Llc Impregnation of a non-conductive material with an intrinsically conductive polymer through in-situ polymerization
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BR112013005537B1 (pt) * 2010-09-07 2021-04-13 Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd Artigo compósito e espuma de nano-material de celulose
BR112016017448B1 (pt) * 2014-01-29 2021-06-08 Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. processo para produção de uma estrutura porosa composta de folhas à base de celulose parcialmente interconectadas, processo para produção de ncc a partir de um material contendo celulose, pó consistindo em fibras de ncc, e solução consistindo em fibras de ncc e pelo menos um solvente
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Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992006239A1 (fr) * 1990-10-09 1992-04-16 Instytut Wlokiennictwa Ameliorations concernant les fibres conductrices
US8012550B2 (en) * 2006-10-04 2011-09-06 3M Innovative Properties Company Ink receptive article
BR112013005537B1 (pt) * 2010-09-07 2021-04-13 Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd Artigo compósito e espuma de nano-material de celulose
US10109386B2 (en) * 2013-05-17 2018-10-23 Heraeus Medical Components Llc Impregnation of a non-conductive material with an intrinsically conductive polymer through in-situ polymerization
CN103641988A (zh) * 2013-11-13 2014-03-19 安徽金马海绵有限公司 一种防静电海绵及其制备方法
BR112016017448B1 (pt) * 2014-01-29 2021-06-08 Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. processo para produção de uma estrutura porosa composta de folhas à base de celulose parcialmente interconectadas, processo para produção de ncc a partir de um material contendo celulose, pó consistindo em fibras de ncc, e solução consistindo em fibras de ncc e pelo menos um solvente
CN109593345A (zh) * 2018-11-26 2019-04-09 重庆工商大学 即时发泡可染色抗静电性能的轻质聚氨酯泡沫的制备方法
CN114953277A (zh) * 2022-06-15 2022-08-30 归壹生命科技(东莞)有限公司 一种泡沫塑料自结皮模具及其生产工艺

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JIA LI JIANG, PHULE AJIT DATTATRAY, GENG YUE, WEN SHIBAO, LI LIN, ZHANG ZHEN XIU: "Microcellular Conductive Carbon Black or Graphene/PVDF Composite Foam with 3D Conductive Channel: A Promising Lightweight, Heat‐Insulating, and EMI‐Shielding Material", MACROMOLECULAR MATERIALS AND ENGINEERING., WILEY VCH VERLAG, WEINHEIM., DE, vol. 306, no. 4, 1 April 2021 (2021-04-01), DE , XP093305446, ISSN: 1438-7492, DOI: 10.1002/mame.202000759 *
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