ES2423256A1 - Automatic and integrated system for the recovery of the fiber and inertization of resin of the preimpregnated carbon fiber (Machine-translation by Google Translate, not legally binding) - Google Patents

Abstract

Integrated process of recovering carbon fiber from prepreg carbon fabric or tape. The process allows the recovery on the one hand of carbon fiber with a practically negligible resin content, and on the other hand of the resin of the polymerized fabric; that is, in the form of inert waste. The process is based on eliminating the partially polymerized resin with a simple process energetically. The process is based on applying heat to decrease the viscosity of the resin; and pressure to make the resin flow. At the end of the process, the polymerized resin and the recycled fiber are separated. In order to achieve a more thorough removal of the resin the process ends with a cleaning with solvent such as acetone. The process is applicable in those cases where the material has expired but the resin has undergone little polymerization so that it can flow when it is overheated and when applying light pressure. In those cases where a more thorough removal of the resin is required, the system allows the coupling of a washing unit with solvent such as acetone. (Machine-translation by Google Translate, not legally binding)

Description

Automatic and integrated system for fiber recovery and inertization of pre-impregnated carbon fiber resin

SECTOR OF THE TECHNIQUE

The patent focuses on a new technology that allows the treatment of expired preimpregnated carbon fabric or tape in the plant for rapid recovery, on the one hand of carbon fiber with a virtually negligible resin content, and on the other of tissue resin polymerized; that is, in the form of an inert residue.

STATE OF THE TECHNIQUE

Traditionally, the components of composite materials of abandoned airplanes and cars at the end of their life cycle have been disposed of in landfills or incinerated. Landfills are the least economically profitable option, in 2004, most of the Member States of the European Union (EU) passed laws prohibiting the dumping of composite materials. On the other hand, regarding incineration, it should be considered that the polymer matrix, like plastics, can release toxic by-products during incineration.

The directive on the end of the vehicle life cycle (EEEV), published in 2000 by the EU, and adopted by the EU member nations in November 2003, requires that 95 percent of all vehicles manufactured after January 2015 must be reused or recovered. There is therefore a political pressure to develop renewable resources, not to mention the growing concern about climate change. As of 2010, the EEEV places the responsibility for the disposal of the original equipment manufacturer (OEM).

Since the idea of recycling composite materials was conceived, the biggest challenge has been to develop a cost-effective recycling process. Technological advances have developed carbon recycling methodologies, obtaining at the end of the recycling process chopped or ground fibers, called short fibers, which prevents their reuse for structural applications. While it is true that the main advantage is its low cost in relation to the cost of continuous fibers.

Currently the demand for short carbon fiber is increasing, especially in applications where the cost savings associated with the reuse of fiber is the main stage while dealing with non-structural applications where the use of short fibers can be a solution. .

Current techniques that allow the carbon fiber to be recycled with thermosetting resin can be classified into three main groups: mechanical, physical and chemical.

Within the mechanical processes we find the crushing to obtain powder or crushed fiber. From recycled powder and fiber by the incorporation of resin, secondary recycle products can be obtained.

The physical methods are mainly thermolysis. That is to say the separation of the resin when it is subjected to a thermal process. In the recycling of carbon fiber the most commonly used type of thermolysis is pyrolysis, degradation of the resin by heating and in the absence of oxygen. Pyrolysis is often performed under vacuum. Heating in a vacuum can reduce the boiling point of the compounds. Pyrolysis and gasification processes are often combined to obtain the energy revaluation of the process.

Chemical methods are generally characterized by providing better quality fibers. In this case, the breakage of the thermostable polymer is induced by the solvent. In addition to solvolysis, carbon fiber recycling has also been proposed through supercritical hydrolysis. In this sense, alcohols have been used both in supercritical and subcritical conditions.

The following table shows the 94 patents most related to the subject. Important to note that none of them performs any treatment similar to that proposed in this patent.

PUBLICATION NUMBER

TITLE  ASSIGNEE-DWPI PUBLICATION YEAR

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58

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KUNSTSTOFF

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TECHNICAL PROBLEM PROPOSED

There is a wide variety of physicochemical procedures that allow the removal of carbon fiber resin and

5 recover the carbon fiber, usually in the form of short fibers, for later use in non-structural parts. It can be said that all the recycling processes described so far treat the expired preimpregnated fabric in the same way as cured carbon fiber parts.

Currently the prepreg carbon fabric is considered dangerous due to the resin and is treated with

10 drastic recycling techniques that eliminate chemical or thermal degradation of the resin. In fact for practical purposes, the expired material reserved in the facilities until it is collected by a specialized waste company, these are the same processes used to recover carbon fiber from cured carbon fiber elements. It is a process that requires great energy.

15 TECHNICAL ADVANTAGE OF THE INVENTION

The main advantage offered by the process is the recovery of fiber at a lower energy cost. Instead of transforming the resin components into volatile compounds at high temperature, the process eliminates the resin by applying pressure and making it flow between the carbon fibers. Finally he undergoes a

20 solvent washing process to remove any resin residue.

EXPLANATION OF THE INVENTION

The proposed recycling process is applicable during the stage that the resin is partially expired

25 polymerized but not completely. So such elimination is a simple energy process. It is based on the fact that during the period that has expired but has not yet fully polymerized, the resin can flow and be removed.

One of the advantages is the recovery of carbon fiber without losing its integrity and maintaining its original length. For this, the process presents a configuration that allows the following actions:

•

Introduction zone of preimpregnated carbon fiber (1)

•

Heating zone of the system to reduce the viscosity of the resin (2)

•

Air inlets and outlets for temperature gradient (7, 8, 9)

•

Resistors (10) and microperforated plates with resistors (11) for temperature increase.

•

Application of moderate pressure to the fibers on the micorperforated plates by means of pressing rollers (12). The resin will pass through the pores and be collected at the bottom to polymerize so that we transform a potential toxic and dangerous product into an inert residue.

•

Vacuum (13) will be applied through the porous plate to suck and help the resin flow. The resin is collected in a lower compartment where it polymerizes to be subsequently treated as an inert residue (14).

•

In the transfer zone between the resin removal zone and the lower zone the resin is superheated to activate its polymerization. The temperature gradient is estimated at about 50 degrees.

•

The fiber passes through a cooling zone, stabilizing the temperature (3)

•

Resin cleaning stage with solvent (4) by means of a drip system (15), resistance (18) and solvent heating (17).

•

The process must contain a drying stage where excess solvent is removed (5).

•

The roll of prepreg fabric located is the carbon inlet coil circulates through the machine where the process to be patented is carried out (16), and at the exit it is rewound (6).

The system is efficient to apply in those cases that the material has expired but that the resin has undergone little polymerization so that it can flow when overheated and when applying light pressure.

In those cases where a more thorough removal of the resin is required, the system allows the coupling of a solvent washing unit such as acetone. Once the fiber has passed through the resin removal zone and has a low resin content, less than 10%, it can be washed in acetone to further reduce the resin content. The resin washing is carried out at a moderate temperature. The acetone cleaning process is similar to going through an acetone bath. This module is sealed with a small stream of air that draws the vapors into a refrigerated trap and through an area of activated carbon filters that prevent the emission of gases and organic compounds.

Claims (15)

one.

The process allows the carbon fiber to be recovered while maintaining its shape and eliminating the thermosetting resin, proceeding with its polymerization and inertization. It is a process applicable to preimpregnated tissue expired but not fully polymerized.

2.

The inertization of the resin is effected by polymerization thereof once separated from the carbon fiber. The resin removal process is the heating of the resin and its fluid promoted by a difference in pressure achieved by applying mechanical pressure on the fiber and vacuum in the resin tank.

3.

A solvent wash, such as acetone, is carried out on the heated material to complete the removal of the last traces of resin, if required by solvent washing such as acetone at moderate temperatures.

Four.

The processed carbon fiber is dried to remove traces of solvent and rolled to recover the tissue in the original carbon dimensions.

5.

The machine has a compact structure so that the machinery defined for the process adapts to rolls of prepreg fabric between 1 and 1.5 m.

6.

To achieve sufficient fluidity of the resin, the system is heated between 90-120 ° C to make the resin flow.

7.

The mechanical pressure exerted on the carbon fiber adapts to the type of fabric and its density. The pressure should be as large as possible to remove most of the resin and be small enough not to cause damage to the fiber.

8.

The mechanical pressure will be exerted by mobile rollers. The rollers must have a polished structure that, using a suitable scraper, any resin residue can be removed by carda.

9.

The resin collected in the polymerization zone of the process is slightly overheated at the interface to promote its polymerization.

10.

The operation of the machine in this process is continuous with all its parts running synchronously.

eleven.

If a solvent cleaning step is incorporated, the carbon with a small resin content and at a suitable temperature is submerged by a solvent bath so that the resin is easily dissolved in the medium.

12.

The solvent can be recovered and reused by a continuous distillation process.

13.

The entire washing zone is sealed and with adequate filtration systems to prevent the release of volatile organic compounds into the environment.

14.

The resin removal modules and the solvent wash module are easily attachable modules.

Figure 1: General Process Outline  ES 2 423 256 Al   Figure 2: Modular configuration of the process and possible machine SPANISH OFFICE OF THE PATENTS AND BRAND Application no .: 201230396 SPAIN Date of submission of the application: 15.03.2012 Priority Date: REPORT ON THE STATE OF THE TECHNIQUE 51 Int. Cl.: See Additional Sheet  RELEVANT DOCUMENTS

Category

56 Documents cited Claims Affected

TO

WO 2012172357 A1 (UNIV NOTTINGHAM), Entire document 1-14

TO

US 2003092783 A (UDAGAWA YOSHITAKA), Entire document 1-14

TO

EP 1160068 B1 (DAIMLER CHRYSLER AG), Entire document 1-14

TO

"Recycling carbon fiber reinforced polymers for structural applications: Technology review andmarket outlook". SORAIA PIMENTA, SILVESTRE T. PINHO.WASTE Management. Volume 31, Issue 2, February 2011, Pages 378–392. 1-14

TO

"Recycling of composite materials". YONGXIANG YANG. Chemical Engineering and Processing: Process Intensification. Volume 51, January 2012, Pages 53–68. 1-14

TO

"Integrated Composite Recycling Process." J-M. GOSAU, T. F. WESLEY, and R. E. ALLRED. Proc. 38th. SAMPE Tech. Conf., Dallas, TX, November 7-9, 2006. 1-14

Category of the documents cited X: of particular relevance Y: of particular relevance combined with other / s of the same category A: reflects the state of the art O: refers to unwritten disclosure P: published between the priority date and the date of priority submission of the application E: previous document, but published after the date of submission of the application

This report has been prepared • for all claims • for claims no:

Date of realization of the report 11.06.2013

Examiner E. Arias Perez-Ilzarbe Page 1/4

REPORT OF THE STATE OF THE TECHNIQUE Application number: 201230396 CLASSIFICATION OBJECT OF THE APPLICATION B29B17 / 02 (2006.01) B29B13 / 02 (2006.01) C08J11 / 06 (2006.01) Minimum documentation sought (classification system followed by classification symbols) B29B, C08J Electronic databases consulted during the search (name of the database and, if possible, terms of search used) INVENTIONS, EPODOC State of the Art Report Page 2/4  WRITTEN OPINION Application number: 201230396 Date of Completion of Written Opinion: 06.11.2013 Statement

Novelty (Art. 6.1 LP 11/1986)

Claims Claims 1-14 IF NOT

Inventive activity (Art. 8.1 LP11 / 1986)

Claims Claims 1-14 IF NOT

The application is considered to comply with the industrial application requirement. This requirement was evaluated during the formal and technical examination phase of the application (Article 31.2 Law 11/1986).  Opinion Base.- This opinion has been made on the basis of the patent application as published. State of the Art Report Page 3/4  WRITTEN OPINION Application number: 201230396  1. Documents considered.- The documents belonging to the state of the art taken into consideration for the realization of this opinion are listed below.

Document

Publication or Identification Number publication date

D01

WO 2012172357 A1 (UNIV NOTTINGHAM) 12/20/2012

D02

US 2003092783 A (UDAGAWA YOSHITAKA) 05.15.2003

D03

EP 1160068 B1 (DAIMLER CHRYSLER AG) 05.12.2001

D04

"Recycling Carbon Fiber reinforced polymers for structural applications: Technology review andmarket outlook". SORAIA PIMENTA, SILVESTRE T. PINHO.WASTE Management. Volume 31, Issue 2, February 2011, Pages 378–392. 02.01.2011

D05

"RECYCLING OF COMPOSITE MATERIALS". YONGXIANG YANG. Chemical Engineering and Processing: Process Intensification. Volume 51, January 2012, Pages 53–68. 01.01.2012

D06

"Integrated Composite Recycling Process." J-M. GOSAU, T. F. WESLEY, and R. E. ALLRED. Proc. 38th. SAMPE Tech. Conf., Dallas, TX, November 7-9, 2006. 09.11.2006

 2. Statement motivated according to articles 29.6 and 29.7 of the Regulation of execution of Law 11/1986, of March 20, on Patents on novelty and inventive activity; quotes and explanations in support of this statement The object of the invention is a process for the recovery of carbon fiber from pre-impregnated fabrics or tapes, which allows the separation on the one hand of the fiber with a very low resin content and on the other of the resin as a residue inert. For this, several treatments are combined: on the one hand a temperature gradient between 90º and 120º is applied combined with a mechanical pressure, and to minimize the resin content in the fibers, they are subjected to a final washing phase with solvents such as acetone. The exponential increase in the use of composite materials in the aeronautical and automotive sectors, as well as the environmental concern has determined the development of various technologies for the recycling and recovery of these materials, which are grouped into three main sections: mechanical, chemical recycling and thermal, the invention being a combination thereof. Although it could be indicated that the basic technology is of thermal type, since initially a temperature gradient is applied through air currents in a range between 90º and 120º. Documents D01 to D07 are those that are considered most representative of the state of the art, and in them various technologies are described. Document D01 describes the treatment of a composite polymeric material (reinforced with carbon fiber) in a fluidized bed at a temperature around 450 °, much higher than the object of the invention. Document D02 starts from a material different from that of the object of the invention (composite material that includes black carbon and rubber) which is subjected to a multi-stage treatment: heating (220º-400), pressure and extraction with a solvent. Although it is a process that combines steps similar to those of the object of the invention, the starting material and the conditions in which they are performed are very different. Document D03 describes the recovery of fibers of a composite material from microwave heating and solvent extraction, but a pressure step is not performed. Documents D04-D06 correspond to bibliographic reviews on the recycling of composite materials, where the different technologies used in this field are analyzed but none of them coincide with the object of the invention. None of the above documents shows a process as claimed in claims 1 to 7. Furthermore, it would not be obvious for a person skilled in the art to conceive a process such as that of the invention, in which a temperature significantly lower than usual is applied. , and therefore claims 1 to 7 are considered to meet the requirements of novelty and inventive height. In the same way, claims 8 to 14, which describe an equipment for carrying out this process, also meet the requirements of novelty and inventive height. State of the Art Report Page 4/4