# US 10,370,459 B2 · Alkyl hydroxyalkyl cellulose ethers, methods of making, and use in cements and mortars

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- Number: US 10,370,459 B2
- Document ID: US10370459B2
- Status: Granted
- Kind: B2
- Application number: 14/338,738
- Filed: 2014-07-23
- Published: 2015-05-28
- Granted: 2019-08-06
- Earliest claimed: 2013-11-25
- Assignees: Hercules Incorporated
- Applicants: Hercules Incorporated
- Inventors: Kelly A. Brush; Patrick J. Cowan; Wilfried Adolphe Hohn; Alexander Adolphe Kindler; Vera Louise Nilles
- Web page: https://patentgrep.com/patent/US10370459B2

## CPC

- C08B 11/08: with hydroxylated hydrocarbon radicals; Esters, ethers, or acetals thereof
- C04B 16/02: Cellulosic materials (cellulosic waste materials, e.g. sawdust, rice husks, C04B18/24)
- C04B 24/383: {Cellulose or derivatives thereof}
- C04B 28/02: containing hydraulic cements other than calcium sulfates
- C08B 11/20: Post-etherification treatments of chemical or physical type, {e.g. mixed etherification in two steps}, including purification
- C04B 2111/00672: {Pointing or jointing materials}
- C08B: POLYSACCHARIDES; DERIVATIVES THEREOF (polysaccharides containing less than six saccharide radicals attached to each other by glycosidic linkages C07H; fermentation or enzyme-using processes C12P19/00; sugar industry C13; production of cellulose D21)
- 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

## Abstract

Disclosed are methods for the preparation of alkyl hydroxyalkyl cellulose ethers, and the use of such alkyl hydroxyalkyl cellulose ethers in the preparation and use of mortars and other cement-based systems; also disclosed is a hydraulic composition containing at least one retarder, at least one accelerator and a cellulose ether having a prolonged open time without deterioration of the other cement tile adhesive properties such as workability, setting time, strength development and sag resistance; and further disclosed are dry mortars containing encapsulated calcium chloride used in preparing mortar materials for use in construction, and the preparation and use of such mortars in cold weather environments is also disclosed.

## Claims

### Claim 1

A method comprising:
a) mixing an alkaline solution comprising an alkali metal hydroxide with cellulose and an alkyl halogenide at a temperature of at least 10° C. to form a first reaction mixture comprising alkali cellulose, water, and the alkyl halogenide, wherein the alkali metal hydroxide is present in an amount of from about 2.92 to about 5.00 equivalents per anhydroglucose unit of the cellulose;
b) adjusting the temperature of the first reaction mixture to be within a range of from about 60 to about 110° C. resulting in a reaction of a portion of the alkyl halogenide with the alkali cellulose forming a second reaction mixture comprising alkyl cellulose ether and unreacted alkyl halogenide, wherein the second reaction mixture is maintained at a temperature within the range of from about 60 to about 110° C. prior to the addition of an alkylene oxide;
c) cooling the second reaction mixture to a temperature in a range of from about 25 to about 80° C. to form a third reaction mixture;
d) adding the alkylene oxide to the third reaction mixture from step c) to form a fourth reaction mixture;
e) adjusting a temperature of the fourth reaction mixture from step d) to be in a range of from about 80 to about 110° C. and reacting at least a portion of the alkyl cellulose ether in the fourth reaction mixture with: i) at least a portion of the alkylene oxide, and ii) at least a portion of the unreacted alkyl halogenide, thereby forming a fifth reaction mixture comprising an alkyl hydroxyalkyl cellulose ether having a methyl D.S. value of from about 1.40 to about 2.10, and a hydroxyethyl M.S. value of from about 0.05 to about 0.4; and
f) recovering the alkyl hydroxyalkyl cellulose ether from the fifth reaction mixture from step e).

### Claim 2 (depends on 1)

The method of claim 1, wherein the alkali metal hydroxide comprises sodium hydroxide.

### Claim 3 (depends on 1)

The method of claim 1, wherein the alkyl halogenide comprises methyl chloride, the alkylene oxide comprises ethylene oxide, and the fifth reaction mixture comprises methyl hydroxyethyl cellulose ether.

### Claim 4 (depends on 1)

The method of claim 1, wherein the first, second, third, fourth, and fifth reaction mixtures each further comprise a diluent.

### Claim 5 (depends on 1)

A process for preparing a wet mortar comprising mixing a dry mixture composition comprising cement, aggregate, and an alkyl hydroxyalkyl cellulose ether prepared by the method of claim 1 with water and thereby applying shear forces.

### Claim 6 (depends on 1)

A process for preparing a mortar comprising the steps of:
a) combining a first dry mixture comprising cement, aggregate, and the alkyl hydroxyalkyl cellulose ether prepared by the method of claim 1 with capsules comprising a CaCl2 compound at least partially coated with a coating material to form a second dry mixture; wherein the CaCl2 compound comprises a compound selected from the group consisting of anhydrous CaCl2, CaCl2•H20, CaCl2•2H2O, CaCl2•4H2O, and combinations thereof; and wherein, on average for the capsules, at least about 70% by weight of the CaCl2 compound surfaces are coated by the coating material;
b) adding water to the second dry mixture thereby forming a water-containing mixture; and
c) mixing the water-containing mixture, thereby applying shear forces to breach the coating material of the capsules to release the CaCl2 compound and form the mortar; wherein the water hydrates the CaCl2 compound resulting in a heat release of at least about 50 kJ/kg of CaCl2 in the CaCl2 compound and thereby raising a temperature of the mortar.

### Claim 7 (depends on 6)

The process of claim 6, wherein the first dry mixture, the second dry mixture, and the water-containing mixture are each at a temperature less than or equal to 15° C.

### Claim 8 (depends on 6)

The process of claim 6, wherein the ambient temperature at which steps b) and c) are performed is less than or equal to 15° C.

### Claim 9 (depends on 6)

The process of claim 6, wherein the time period for hydration of the cement in the mortar is reduced as compared to the time period for hydration of cement in an identical mortar not prepared using the capsules.

### Claim 10 (depends on 6)

The process of claim 6, wherein the average particle size of the capsules is less than or equal to 5 mm.

### Claim 11 (depends on 6)

The process of claim 6, wherein the coating material is hydrophobic.

### Claim 12 (depends on 6)

The process of claim 6, wherein the mortar is cured to form a cured mortar, and wherein the cured mortar has a compressive strength higher than the compressive strength of an identical cured mortar not prepared using the capsules.

### Claim 13 (depends on 6)

The process of claim 6, wherein the mortar is cured to form a cured mortar, and wherein the cured mortar has a flexural strength higher than the flexural strength of an identical cured mortar not prepared using the capsules.