Preparation method of aminated thiolignin-based strong oil absorption material

A technology of aminated lignin and lignin-based, which is applied in the field of preparation of oil-absorbing materials, can solve the problems of poor surface activity of modified lignin amine, low three-dimensional network chemical cross-linking structure, water absorption and oil absorption performance interference, etc. Achieve the effect of uncomplicated treatment method, simple recycling process and low cost

Inactive Publication Date: 2017-06-20
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional resin oil-absorbing materials are acrylic resins and olefin resin materials, and their structures are characterized by low three-dimensional network chemical cross-linking structures. There is a problem of competitive adsorption between water and oil in the treatment of oil pollution on the sea surface caused by oil spills from tankers. , resulting in mutual interference of water absorption and oil absorption
In the prior art, Chinese Journal of Papermaking. 2005, 20 (2): 75-78 discloses that a conventional heating reaction has been used to synthesize diethylenetriamine / formaldehyde modified lignin amine, and it is found that it is used as a co-emulsifier, which is effective on asphalt. Emulsification has an auxiliary effect, but due to the poor surface activity of modified lignin amine, it cannot be directly used in oil-absorbing materials
The Chinese patent with the publication number CN 104448340A discloses a lignin-based microporous molecular sieve composite oil-absorbing material, which can be used to solve the problem of low primary oil absorption by virtue of the advantages of regular molecular sieve channels and controllable pore size distribution. Synthesis, silylation, and copolymerization are prepared in three steps. The synthetic route is long and the product yield is not high, resulting in complicated process and high cost.

Method used

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  • Preparation method of aminated thiolignin-based strong oil absorption material
  • Preparation method of aminated thiolignin-based strong oil absorption material
  • Preparation method of aminated thiolignin-based strong oil absorption material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take a 250mL three-necked flask, dissolve 20g of lignin (about 0.1mol according to the C9 unit, the same below) in 50mL of NaOH solution (concentration 1mol / L), stir well, put it into a microwave reactor, set the temperature to 40 Under the conditions of ℃, reaction pressure 1MPa, microwave power 400W, heat up to the preset temperature, add 0.1mol of aminating agent diethylenetriamine (DETA), then slowly drop 5mL (about 0.1mol) of 37wt% formaldehyde solution, reflux and stir , so that the active hydrogen of the methoxy group on the lignin, the active oxygen on the formaldehyde, and the active hydrogen connected to the nitrogen on the aminating agent take place Mannich reaction (Mannish reaction), after the insulation reaction for 20 minutes, the reaction solution is poured into 80 In hot distilled water at ℃, add 1mol / L hydrochloric acid solution dropwise under stirring to fully separate the aminated lignin, let it stand for 3 hours, filter, wash with 0.1mol / L dilute hyd...

Embodiment 2

[0029] Aminated lignin A was prepared as in Example 1. Take 4g of vulcanizing agent CS2 (0.1mol) and slowly add it to the suspension of aminated lignin A (mass concentration 10%) dissolved in pyridine solvent, wherein the molar ratio of CS2 to aminated lignin B is about 1:1.40 The reaction was stirred and reacted at ℃ for 48 hours, and the product was cooled to room temperature, filtered, washed with ethanol solvent, washed with distilled water, and dried at 80℃ for 5 hours to obtain a solid substance which was a thioaminated lignin-based strong oil-absorbing material B (mass yield 97.3% ).

[0030] The commercial oil-absorbing resin materials butyl acrylate and octadecyl acrylate polymer were used as the control sample C to carry out the chloroform adsorption test experiment, and 0.1g of the above-mentioned composite oil-absorbing material B and control sample C were weighed and placed in a 100mL grinding mouth drying cone Add 50mL of distilled water to soak in a shaped bott...

Embodiment 3

[0032] Aminated lignin A was prepared as in Example 1, wherein the reaction conditions were changed to temperature 60° C., reaction pressure 0.5 MPa, microwave power 600 W, and reaction time 10 minutes to obtain aminated lignin A (mass yield 88.9%). Take 8 g of vulcanizing agent CS2 (0.2 mol) and slowly add it to the suspension of aminated lignin A (mass concentration 10%) dissolved in pyridine solvent, wherein the molar ratio of CS2 to aminated lignin B is about 2:1.40 Stir the reaction at ℃ for 48 hours, wait for the product to cool to room temperature, filter, wash with ethanol solvent, wash with distilled water, and dry at 80℃ for 5 hours to obtain a solid substance which is a thioaminated lignin-based strong oil-absorbing material B (mass yield 89.4% ).

[0033] The commercial oil-absorbing resin materials butyl acrylate and octadecyl acrylate polymer were used as the control sample C to carry out the chloroform adsorption test experiment, and 0.1g of the above-mentioned ...

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Abstract

The invention discloses a preparation method of an aminated thiolignin-based strong oil absorption material. The preparation method is simple, is low in energy consumption, and is wide in application range. The obtained aminated thiolignin-based strong oil absorption material is high in oil absorption rate. The preparation method comprises following steps: lignin is dissolved in a NaOH aqueous solution, an amination agent is added after full stirring, a formaldehyde solution is added slowly, thermal insulation reaction is carried out for 15min to 2h, an obtained reaction solution is added into heat distilled water, hydrochloric acid is added dropwise with stirring so as to realize full precipitation of aminated lignin, the aminated lignin is washed until pH value of a washing solution is increased to be 7, is dried, is grinded into fine powder, and then is subjected to vacuum drying so as to obtain aminated lignin; at 25 to 45 DEG C, a vulcanizing agent is added into an aminated lignin suspension obtained via dissolving of aminated lignin in a solvent, stirring reaction is carried out for 24 to 72h at 25 to 45 DEG C, and an obtained product is cooled to room temperature, is filtered, is washed with distilled water, and is dried so as to obtain a solid product which is the aminated thiolignin-based strong oil absorption material.

Description

technical field [0001] The invention relates to a preparation method of an oil-absorbing material, in particular to a preparation method of a thioaminated lignin-based strong oil-absorbing material. Background technique [0002] Lignin is a complex multi-ring structure and three-dimensional network polymer organic matter (see the following formula). There are functional groups such as alcoholic hydroxyl group (a), phenolic hydroxyl group (b), carboxyl group, and methoxyl group on the molecule, which are beneficial to the macromolecular structure. grooming. In nature, the reserve of lignin is second only to cellulose, and it is regenerated at a rate of tens of billions of tons every year. The pulp and paper industry separates about 140 million tons of cellulose from plants every year, and at the same time obtains about 50 million tons of lignin by-products, but so far, more than 95% of lignin has been directly discharged into rivers as "black liquor". It causes serious seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F101/36
CPCB01J20/24B01J2220/4837C02F1/286C02F2101/36
Inventor 顾晓利吴志鹏周徐亮姚丽君姚建峰何明罗振扬
Owner NANJING FORESTRY UNIV
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