Deodorized rosin ester and methods for making

Patent metadata

Field	Value
Publication number	US-11279849-B2
Application number	US-202015929780-A
Country	US
Kind code	B2
Filing date	May 21, 2020
Priority date	May 21, 2020
Publication date	Mar 22, 2022
Grant date	Mar 22, 2022

Abstract

A process for deodorizing a rosin ester composition is disclosed. The process employs an adsorptive bed containing an adsorbent material. The adsorbent material comprises silica adsorbent having an average pore size between 50-200 Å, BET surface area of at least 300 m2/g, pore volume of 1.20 to 3.00 cc/g, and a silanol [Si—OH] level of 0.5 to 5 unit/nm2. The deodorized rosin ester composition has an odor intensity reduction of at least 1 unit on odor intensity scale of Offensive Odor Control Act as compared to the rosin ester feedstock. In embodiment, the deodorizing treatment comprises using multi-staged adsorbent system with an adsorbent column having multiple layers of different adsorbent materials.

First claim

The invention claimed is:

1. A process for deodorizing a rosin ester composition, the process comprising:
providing a rosin ester feedstock in a liquid form by dissolving a solid rosin ester in a solvent, the rosin ester feedstock having a viscosity in a range of 5-150 cPs, an initial color, and an odor intensity;
contacting the rosin ester feedstock with an adsorbent material in an adsorbent bed, obtaining a deodorized rosin ester composition;
wherein the solvent is present in the rosin ester feedstock in an amount of at least 35 wt. % based on the total weight of the rosin ester feedstock;
wherein the adsorbent bed is operated at an adsorption temperature of 20-30° C., and at one bar pressure;
wherein the adsorbent material comprises silica adsorbent having an average pore size between 50-200 Å, BET surface area of at least 300 m 2 /g, pore volume of 1.20 to 3.00 cc/g, and a silanol [Si—OH] level of 0.5 to 5 unit/nm 2 ; and

wherein the deodorized rosin ester composition has an odor intensity reduction of at least 1 unit on odor intensity scale of Offensive Odor Control Act as compared to the rosin ester feedstock.

2. The process of claim 1 , wherein the deodorized rosin ester composition has an odor intensity reduction of at least 2 units as compared to the rosin ester feedstock.

3. The process of claim 2 , wherein the deodorized rosin ester composition has an odor intensity reduction of at least 3 units as compared to the rosin ester feedstock.

4. The process of claim 1 , wherein the adsorbent bed is operated at a superficial velocity (V) of at least 0.3 ft/hr.

5. The process of claim 4 , wherein the adsorbent bed is operated at a superficial velocity (V) of at least 1 ft/hr.

6. The process of claim 1 , wherein the deodorized rosin ester composition has a reduction in color of at least 1 Gardner number as compared to the initial color of the rosin ester feedstock.

7. The process of claim 6 , wherein the deodorized rosin ester composition has a reduction in color of at least 2 Gardner numbers.

8. The process of claim 1 , wherein 35-65 wt. % of the solid rosin ester is dissolved in the solvent, based on the total weight of the rosin ester and the solvent.

9. The process of claim 8 , further comprising recovering the deodorized rosin ester by evaporating the solvent.

10. The process of claim 1 , wherein 40-55 wt. % of the solid rosin ester is dissolved in the solvent, based on the total weight of the rosin ester and the solvent.

11. The process of claim 1 , wherein the solvent is selected from alcohols, ethers, ketones, esters, tertiary amides, aliphatic hydrocarbons, aromatic hydrocarbons, and mixtures thereof.

12. The process of claim 1 , wherein the solvent is selected from hexanes, heptanes, petroleum ether, cyclohexane, dipentane, napthal, mineral spirts, toluene, pentane, and mixtures thereof.

13. The process of claim 1 , further comprising
collecting the adsorbent material, and
passing a solvent over the adsorbent material in the adsorbent bed, for a sufficient period of time, to dissolve odor causing species and regenerate the adsorbent material.

14. The process of claim 13 , wherein the solvent used for regenerating the adsorbent material is selected from methanol, ethanol, acetone and mixtures thereof.

15. The process of claim 1 , wherein the adsorbent bed comprises a multi-stage adsorbent column having at least two layers, each layer with a different adsorbent material.

16. The process of claim 1 , wherein the adsorbent bed comprises at least two different adsorbent columns, with each adsorbent column containing different adsorbent material.

17. A process for deodorizing a rosin ester composition, the process comprising:
providing a rosin ester feedstock in a liquid form by dissolving a solid rosin ester in a solvent, the rosin ester feedstock having a viscosity in a range of 5-150 cPs;
contacting the rosin ester feedstock with two adsorbent beds in series, a first adsorbent bed containing a first adsorbent material and a second adsorbent bed containing a second adsorbent material, obtaining a deodorized rosin ester composition,
wherein the first adsorbent material and the second adsorbent material are different,
wherein at least one of the first adsorbent material and the second adsorbent material is a silica adsorbent having an average pore size between 50-200 Å, a BET surface area of at least 300 m 2 /g, pore volume of 1.20 to 3.00 cc/g, and a silanol [Si—OH] level of 0.5 to 5 unit/nm 2 ;
wherein the solvent is present in the rosin ester feedstock in an amount of at least 30 wt. % based on the total weight of the rosin ester feedstock;
wherein at least one of the adsorbent beds is operated at an adsorption temperature of 20-30° C., and at one bar pressure; and
wherein the deodorized rosin ester composition has an odor intensity reduction of at least 2 units on odor intensity scale of Offensive Odor Control Act as compared to the rosin ester feedstock.

18. The process of claim 17 , wherein the first adsorbent bed and the second adsorbent bed are in a single adsorption column having different layers of adsorbent materials.

Assignees

• Kraton Polymers Llc

Inventors

• Tian Jason
• Ding Ruidong
• Reiter Chad

Classifications

• C09F1/04 Primary

  Chemical modification, e.g. esterification (resin soaps C11D) · CPC title

• C09F1/02

  Purification · CPC title

• B01J20/28061

  being in the range 100-500 m2/g · CPC title

• B01J20/28076

  being more than 1.0 ml/g · CPC title

• B01J20/103 Primary

  comprising silica · CPC title