Method for preparing amphiphilic lignin nanomaterial based on pulping black liquor, amphiphilic lignin nanomaterial, and oil sludge detergent

Patent metadata

Field	Value
Publication number	US-11731997-B2
Application number	US-202017095297-A
Country	US
Kind code	B2
Filing date	Nov 11, 2020
Priority date	Nov 11, 2020
Publication date	Aug 22, 2023
Grant date	Aug 22, 2023

Abstract

The disclosure provides a method for preparing an amphiphilic lignin nanomaterial based on pulping black liquor, an amphiphilic lignin nanomaterial, and an oil sludge detergent. In the disclosure, physical treatments such as ball milling and high-pressure jet homogenization treatment are conducted on alkali lignin at the early stage to adjust the molecular weight and size of alkali lignin and thus to give alkali lignin nanoparticles with uniform particle sizes; and on this basis, a chemical treatment such as alkylation grafting modification is conducted to give amphiphilic lignin nanoparticles with both hydrophilicity and lipophilicity. Due to the nano-size effect, the amphiphilic lignin nanomaterial has a significantly-increased specific surface area (SSA) and effectively-improved surface properties, which can reduce the oil-water interfacial tension, and emulsify the crude oil and peel off the crude oil from the surface of rock particles, so as to achieve the purpose of oil-solid separation.

First claim

What is claimed is:

1. A method for preparing an amphiphilic lignin nanomaterial based on pulping black liquor, comprising the following steps:
subjecting pulping black liquor to acid precipitation, solid-liquid separation and ball milling to give alkali lignin particles;
mixing the alkali lignin particles, a hydrogen peroxide solution and water to give an activation treatment solution; and subjecting the activation treatment solution sequentially to activation treatment and microjet homogenization treatment to give activated alkali lignin nanoparticles;
mixing the activated alkali lignin nanoparticles, Na 2 SO 3 , HCHO and deionized water to give a sulfonation treatment solution, and subjecting the sulfonation treatment solution to sulfomethylation modification to give hydrophilic lignosulfonate nanoparticles; and
mixing the hydrophilic lignosulfonate nanoparticles, long-chain alkylene oxide and i-propanol to give a chemical grafting treatment solution, and subjecting the chemical grafting treatment solution to chemical grafting to give an amphiphilic lignin nanomaterial.

2. The method according to claim 1 , wherein, the pH for the acid precipitation is 2 to 3.

3. The method according to claim 1 , wherein, the ball milling is conducted under the following parameters: volume fraction of filler in the ball milling tank: 20% to 25%; ball-to-material ratio: (3-6):1; rotational speed: 400 r/min to 500 r/min; and ball milling time: 4 h to 8 h.

4. The method according to claim 1 , wherein, in the activation treatment solution, the alkali lignin particles have a mass concentration of 5 g/L to 10 g/L; the hydrogen peroxide solution with a mass concentration of 30% has a volume fraction of 0.2% to 0.5%; and the activation treatment is conducted at 55° C. to 65° C. for 0.2 h to 1 h.

5. The method according to claim 1 , wherein, the microjet homogenization treatment is conducted under pressure of 30 MPa to 50 MPa.

6. The method according to claim 4 , wherein, the microjet homogenization treatment is conducted under pressure of 30 MPa to 50 MPa.

7. The method according to claim 1 , wherein, in the sulfonation treatment solution, Na 2 SO 3 has a mass fraction of 0.1% to 0.4%; HCHO has a volume fraction of 0.2% to 0.5%; the activated alkali lignin nanoparticles have a mass concentration of 10 g/L; and the sulfomethylation modification is conducted at 70° C. to 120° C. for 1 h to 4 h.

8. The method according to claim 1 , wherein, in the chemical grafting treatment solution, the hydrophilic lignosulfonate nanoparticles have a mass concentration of 10 g/L; the long-chain alkylene oxide has a volume fraction of 0.2% to 1.0%; and the long-chain alkylene oxide is 2-epoxypropyl dodecyl dimethyl ammonium chloride or 3-chloro-2-hydroxypropyl dimethyl octadecyl ammonium chloride.

9. The method according to claim 1 , wherein, the chemical grafting is conducted at 50° C. to 60° C. for 1 h to 2 h, with a pH of 10 to 12.

10. The method according to claim 8 , wherein, the chemical grafting is conducted at 50° C. to 60° C. for 1 h to 2 h, with a pH of 10 to 12.

11. An amphiphilic lignin nanomaterial obtained by the method according to claim 1 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

12. An amphiphilic lignin nanomaterial obtained by the method according to claim 2 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

13. An amphiphilic lignin nanomaterial obtained by the method according to claim 3 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

14. An amphiphilic lignin nanomaterial obtained by the method according to claim 4 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

15. An amphiphilic lignin nanomaterial obtained by the method according to claim 5 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

16. An amphiphilic lignin nanomaterial obtained by the method according to claim 6 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

17. An amphiphilic lignin nanomaterial obtained by the method according to claim 7 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

18. An amphiphilic lignin nanomaterial obtained by the method according to claim 8 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

19. An amphiphilic lignin nanomaterial obtained by the method according to claim 9 , wherein, the amphiphilic lignin nanomaterial has a particle size of 20 nm to 100 nm.

20. An oil sludge detergent, comprising the following components, in mass percentage: 1% to 5% of the amphiphilic lignin nanomaterial according to claim 11 , 0.2% to 2% of surfactant, 1% to 1.2% of inorganic salt, and the balance of water, wherein, the surfactant is octylphenol polyoxyethylene ether and/or nonylphenol polyoxyethylene ether; and the inorganic salt comprises one or more of sodium chloride, sodium carbonate and magnesium chloride.

Assignees

• Univ Guangxi

Inventors

• Qin Chengrong
• Zhang Jian
• Liang Chen
• Yao Shuangquan
• Liu Xinliang
• Wang Zhiwei
• Li Wei
• Sha Jiulong

Classifications

• C11D2111/24

  Mineral surfaces, e.g. stones, frescoes, plasters, walls or concretes · CPC title

• C07G1/00 Primary

  Low-molecular-weight derivatives of lignin (high-molecular-weight derivatives of lignin {C08H6/00}) · CPC title

• B01F23/511

  characterised by the composition of the liquids or solids · CPC title

• B01F23/54

  wetting solids · CPC title

• B01F23/59

  Mixing systems, i.e. flow charts or diagrams · CPC title