# US 10,119,026 B2 · Additive for asphalt mixes containing reclaimed bituminous products

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- Number: US 10,119,026 B2
- Document ID: US10119026B2
- Status: Granted
- Kind: B2
- Application number: 14/348,916
- Filed: 2012-10-12
- Published: 2014-08-21
- Granted: 2018-11-06
- Earliest claimed: 2011-10-12
- Assignees: Arkema France
- Applicants: Ceca S.A.
- Inventors: Juan Antonio Gonzalez Leon; Gilles Barreto; Vincent Luca
- Web page: https://patentgrep.com/patent/US10119026B2

## CPC

- C08L 95/00: Compositions of bituminous materials, e.g. asphalt, tar, pitch
- C04B 26/006: {Waste materials as binder}
- C04B 26/26: Bituminous materials, e.g. tar, pitch {(C08L95/00 takes precedence)}
- C04B 40/0039: {Premixtures of ingredients}
- C08K 5/3445: Five-membered rings
- C08K 5/36: Sulfur-, selenium-, or tellurium-containing compounds {(C08K5/0091 takes precedence)}
- C08K 5/52: Phosphorus bound to oxygen only
- C04B 2111/0075: {for road construction}
- C08L 2555/34: Recycled or waste materials, e.g. reclaimed bitumen, asphalt, roads or pathways, recycled roof coverings or shingles, recycled aggregate, recycled tires, crumb rubber, glass or cullet, fly or fuel ash, or slag
- Y02W 30/91: Use of waste materials as fillers for mortars or concrete
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- Y02W: CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT

## Abstract

The present invention relates to a method of improving the incorporation of recycled bituminous products by using at least one surfactant as an alternative to the known rejuvenating oils, for the preparation of asphalt mixes containing recycled bituminous products. The use of such alternative surfactant(s) results in better mechanical properties of the asphalt mix, while using smaller amounts of fresh bitumen and greater amounts of recycled bituminous products.

## Claims

### Claim 1

A process for the preparation of an asphalt mix comprising a fraction of at least one recycled bituminous product, which comprises mixing the at least one recycled bituminous product including RAP or RAS with at least one non-ionic or cationic surfactant, present in amounts that range from 0.05 wt % to 10 wt % with respect to the total mass of bitumen present in the final asphalt mix, such that the at least one surfactant is directly added to the at least one recycled bituminous product and results in improved mechanical properties of the mix, when present, and obtaining the asphalt mix, wherein the asphalt mix is free of rejuvenating oil, the surfactant amount facilitates the mixing of the aged binder present in recycled bituminous products with fresh bitumen used in the preparation of asphalt mixes, and the fraction of recycled bituminous product(s) is present in amounts from about 5 wt % to 99.5 wt % of the total mass of the final asphalt mix.

### Claim 2 (depends on 1)

The process according to claim 1, further comprising the following steps of:
providing fresh bitumen and optionally fresh aggregates to the mixture of the at least one recycled bituminous product and the at least one surfactant, and
mixing the fresh bitumen and the optional fresh aggregates with the at least one recycled bituminous product and the at least one surfactant after the at least one recycled bituminous product is mixed with the at least one surfactant.

### Claim 3 (depends on 2)

The process of claim 2, wherein the fresh bitumen is supplied in a content of from about 2 percent to about 5.5 percent.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the at least one recycled bituminous product is chosen from among reclaimed asphalt pavement, waterproof membranes, bituminous shingles, sound-proof panels, wastes resulting from production of the reclaimed asphalt pavement, waterproof membranes, bituminous shingles, and sound-proof panels, and mixtures of two or more thereof.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the fraction of recycled bituminous product(s) represents from about 10 wt % to about 80 wt % of the total mass of the final asphalt mix.

### Claim 6 (depends on 5)

The process of claim 5, wherein the fraction of recycled bituminous product(s) represents from about 12 wt % to about 50 wt %.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the at least one surfactant is chosen from among non-ionic and cationic surfactants, and comprises 2 or more identical or different heteroatoms, said heteroatoms being chosen from among nitrogen, oxygen, phosphor and sulfur.

### Claim 8 (depends on 7)

The process of claim 7, wherein the at least one surfactant is chosen from among non-ionic surfactants.

### Claim 9 (depends on 7)

The process of claim 7, wherein the at least one surfactant comprises more than two identical or different heteroatoms.

### Claim 10 (depends on 7)

The process of claim 7, wherein the at least one surfactant comprises at least two heteroatoms which are different from one another.

### Claim 11 (depends on 1)

The process according to claim 1, wherein the at least one surfactant is of formula A1:
[A-O—B-]dZ (A1)
wherein:
A is chosen from hydrogen, a group G, or
G represents a linear or branched, saturated or unsaturated, C1-C30 hydrocarbon chain, optionally containing at least one aromatic cycle, and optionally substituted by at least one phosphate group,
B represents a bond or a divalent group containing at least one alkylene oxide repeating unit,
d represents 1 or 2, and
Z represents a radical of formula Z1 or Z2:
wherein R is hydrogen or a linear or branched C1-C6 alkyl, f is 0 or 1 or 2, e is 0 or 1, and d+e+f is 3,
provided that when d is 2, then Z is Z1, e is 0 and P is linked to two identical or different groups [A-O—B—], and
provided that in the case where d is 1, Z may also represent hydrogen or a group G or

### Claim 12 (depends on 11)

The process of claim 11, wherein G represents a linear or branched, saturated or unsaturated, C1-C30 hydrocarbon chain, optionally containing at least one aromatic cycle, and optionally substituted by one phosphate group.

### Claim 13 (depends on 11)

The process of claim 11, wherein Z represents a radical of formula Z1.

### Claim 14 (depends on 11)

The process of claim 11, wherein when d is 2, then Z is Z1, e is 0 and P is linked to two identical groups [A-O—B—].

### Claim 15 (depends on 1)

The process according to claim 1, wherein the at least one surfactant is of formula E1:
(E)j-Y (E1)
E is chosen from among G,
G represents a linear or branched, saturated or unsaturated, C1-C30 hydrocarbon chain, optionally containing at least one aromatic cycle, and optionally substituted by at least one phosphate group,
j represents 1 or 2, and
R′ is chosen from among HO—, Q-O— and Q, wherein Q is a linear or branched C1C6 alkyl radical,
Y represents a group chosen from among —O-T, —S-T, —N(H)(2-j)-T, and —NT1T2, provided that Y is not —S-T, when E is bound to Y via a sulfur atom,
T represents hydrogen or a linear, branched or cyclic or cyclic-containing moiety having carbon and hydrogen atoms, and optionally one or more heteroatoms chosen from among nitrogen, oxygen, sulfur and phosphorus,
T1 and T2, identical or different have the same meaning as for T above, or T1 and T2, together with the nitrogen atom to which they are bonded, represent a saturated, partially saturated or unsaturated heterocycle, optionally further comprising one or more heteroatoms chosen from among nitrogen, oxygen, sulfur and phosphorus.

### Claim 16 (depends on 15)

The process according to claim 15, wherein the at least one surfactant is chosen from compounds of formula E1C, E1D and E1E, wherein G is a C14-C22, linear, saturated or partially unsaturated hydrocarbon chain:

### Claim 17 (depends on 15)

The process of claim 15, wherein G represents a linear or branched, saturated or unsaturated, C1-C30 hydrocarbon chain, optionally containing at least one aromatic cycle, and optionally substituted by one phosphate group.

### Claim 18 (depends on 15)

The process of claim 15, wherein Y represents —N(H)(2-j-T or —NT1T2.

### Claim 19 (depends on 16)

The process of claim 16, wherein G is a C14-C22 partially unsaturated hydrocarbon chain.

### Claim 20 (depends on 1)

The process according to claim 1, further comprising, after the step of mixing the at least one recycled bituminous product with the at least one surfactant, a step of mixing the at least one recycled bituminous product and the at least one surfactant with mineral aggregates, water, optionally a breaking control additive, and an emulsion of virgin bitumen.

### Claim 21 (depends on 1)

The process according to claim 1, wherein the process is carried out free of water.

### Claim 22 (depends on 1)

The process according to claim 1, comprising a further step consisting in adding one or more other additives, chosen from among:
polyphosphoric acid, comprising all different existing grades and designations of polyphosphoric acids including pyrophosphoric acid, triphosphoric and metaphosphoric acids with phosphonic acid,
pyrophosphates, and other similar compounds comprising at least one (OH—)P═O group,
polymers,
waxes,
fluxants,
organic or inorganic acids,
esters of fatty acids and functionalized waxes,
resin components,
asphaltites,
organic fibers and/or inorganic fibers,
as well as mixtures of two or more of the above additional additives.

### Claim 23 (depends on 22)

The process of claim 22, wherein the waxes comprise Fischer-Tropsch waxes.

### Claim 24 (depends on 1)

The process of claim 1, wherein the amount of surfactant ranges from 0.1 wt % to 5 wt %.

### Claim 25 (depends on 24)

The process of claim 24, wherein the amount of surfactant ranges from 0.1 wt % to 2.5 wt % with respect to the total mass of bitumen present in the final asphalt mix.

### Claim 26 (depends on 1)

The process of claim 1, wherein the fraction of recycled bituminous product(s) represents from about 10 wt % to about 99 wt %.

### Claim 27 (depends on 26)

The process of claim 26, wherein the fraction of recycled bituminous product(s) represents from about 35 wt % to about 99 wt %.

### Claim 28 (depends on 27)

The process of claim 27, wherein the fraction of recycled bituminous product(s) represents from about 40 wt % to about 99 wt %.

### Claim 29 (depends on 1)

The process of claim 1, wherein the at least one surfactant is a non-ionic surfactant.

### Claim 30 (depends on 1)

The process of claim 1, wherein the step of mixing results in a decrease of fresh bitumen content, at which maximum stability of the asphalt mix is observed, by as much as 80 wt %.

### Claim 31 (depends on 1)

The process of claim 1, wherein, over a fresh bitumen content of 3 percent to 5.5 percent, the improved mechanical property is indirect tensile strength (“ITS”) value of about 2.25 MPa.

### Claim 32 (depends on 1)

The process of claim 1, wherein the amount of surfactant ranges from 0.8 wt % to 10 wt % with respect to the total mass of bitumen present in the final asphalt mix.

### Claim 33

A process for the preparation of an asphalt mix comprising a fraction of at least one recycled bituminous product including RAP or RAS, which comprises mixing at least one non-ionic or cationic surfactant, present in amounts that range from 0.05 wt % to 10 wt % with respect to the total mass of bitumen present in the final asphalt mix, with the at least one recycled bituminous product such that the at least one surfactant is directly added to the at least one recycled bituminous product, and the asphalt mix is free of rejuvenating oil, and mixing the at least one surfactant and the at least one recycled bituminous product from the first mixing step with fresh bitumen, wherein the fresh bitumen content is less than 5.5 percent and the fraction of recycled bituminous product(s) is present in amounts from about 5 wt % to 99.5 wt % of the total mass of the final asphalt mix.

### Claim 34 (depends on 33)

The process of claim 33, which results in a decrease of fresh bitumen content, at which maximum stability of the asphalt mix is observed, by as much as 80 wt %.

### Claim 35

A process for the preparation of an asphalt mix comprising a fraction of at least one recycled bituminous product including RAP or RAS, which comprises mixing the at least one recycled bituminous product with at least one non-ionic or cationic surfactant such that the at least one surfactant, present in amounts that range from 0.05 wt % to 10 wt % with respect to the total mass of bitumen present in the final asphalt mix, is directly added to the at least one recycled bituminous product, wherein the at least one surfactant results in improved mechanical properties of the mix, and the surfactant amount facilitates the mixing of the aged binder present in recycled bituminous products with fresh bitumen used in the preparation of asphalt mixes and the fraction of recycled bituminous product(s) is present in amounts from about 5 wt % to 99.5 wt % of the total mass of the final asphalt mix, and obtaining the asphalt mix, wherein the asphalt mix is free of rejuvenating oils selected from the group consisting of aliphatic oils, fatty acids, fatty acid esters, and synthetic and natural phenolic compounds.