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Preparation method of ether bond connected multi-carboxyl modified regenerated cellulose

A technology of regenerated cellulose and carboxyl group modification, applied in plant fiber, fiber treatment, textile/flexible product manufacturing, etc., can solve the problems of inability to be used as heavy metal ion adsorbent, increased water solubility of cellulose powder, poor tolerance, etc. Achieve the effects of low processing cost, high stability and adsorption capacity, and easy industrialization

Active Publication Date: 2021-08-10
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Literature "Zhang Kai, Li Zongjie, Deng Nanping, et al. Tree-likecellulose nanofiber membranes modified by citric acid for heavy metal ion (Cu 2 + )removal[J].Cellulose,2019,26(2):945-958"introduced polycarboxylates into cellulose by citric acid modification, but the reaction was carried out under high temperature and high pressure conditions, and citric acid and Cellulose is connected by ester bonds, and has poor resistance to higher acid and alkaline environments
In the document "Ricardo Chagas, Martin Gericke, Ricardo B. Ferreira, et al. Synthesis and characterization of dicarboxymethyl cellulose [J]. Cellulose, 2020, 27: 1965-1974", sodium bromomalonate was used to carboxylate cellulose powder Modification, but sodium bromomalonate is a non-commercialized product, and as the degree of substitution of hydroxyl groups in cellulose increases, the water solubility of cellulose powder will increase, so it cannot be used as an adsorbent for heavy metal ions

Method used

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  • Preparation method of ether bond connected multi-carboxyl modified regenerated cellulose
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  • Preparation method of ether bond connected multi-carboxyl modified regenerated cellulose

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preparation example Construction

[0026] The present invention provides a kind of preparation method (abbreviation method) of polycarboxy-modified regenerated cellulose linked by ether bond, it is characterized in that, the method comprises the following steps:

[0027] Step 1, adding the cellulose acetate product to an excessive amount of strong alkaline solution, carrying out saponification reaction under stirring conditions to change the ester group of the cellulose acetate into a hydroxyl group to obtain a regenerated cellulose product;

[0028] Preferably, in step 1, the cellulose acetate product is cellulose acetate film, cellulose acetate nonwoven fabric, cellulose acetate fiber or cellulose acetate resin;

[0029] Preferably, in step 1, the strong alkaline solution is sodium hydroxide solution, potassium hydroxide solution or calcium hydroxide solution, preferably sodium hydroxide solution;

[0030] Preferably, in step 1, the obtained regenerated cellulose product is washed to neutrality through deioni...

Embodiment 1

[0052] (1) Spinning cellulose acetate nano-micron fiber membrane: multi-needle electrospinning equipment is used to spin the fiber membrane, wherein the mass fraction of cellulose acetate in the spinning solution is 19%, and the soluble volume ratio is 2: 1 in N,N-dimethylformamide / acetone mixed solvent; the spinning solution forms fibers at a liquid feeding rate of 0.6mL / h at a spinning voltage of 20kV, 25°C and 70% ambient humidity, and the spinning needle Make a reciprocating motion along the radial direction of the receiving roller at a horizontal distance of 10 cm from the grounded receiving roller, and the cellulose acetate nano-micron fiber film can be received on the surface of the roller, and vacuum-dried at 50 ° C for 48 hours for later use;

[0053] (2) Preparation of regenerated cellulose nano-micron fiber membrane: immerse 0.25 g of dry cellulose acetate nano-micron fiber membrane in 100 ml of aqueous sodium hydroxide solution with a concentration of 0.5 mol / L, car...

Embodiment 2

[0060] Steps (1), (2) and (4) of this example are the same as steps (1), (2) and (4) of Example 1 respectively, and the etherification grafting reaction time of step (3) is 3h.

[0061] Depend on Figure 4 It can be seen that the fiber structure of the membrane after saponification reaction and 3h etherification grafting modification reaction has not been damaged.

[0062] Depend on Figure 5 It can be seen that compared with Comparative Example 2, the infrared spectrogram is at 1730cm -1 A new characteristic absorption peak appeared at (-COOH), indicating that the alkali-catalyzed etherification reaction was successfully completed on the surface of the regenerated cellulose nanofiber membrane, and polycarboxylic groups were introduced into the regenerated cellulose.

[0063] Adsorption test of heavy metal ions, polyvalent carboxyl-modified regenerated cellulose nanofiber membranes linked by ether bonds to Cu 2+ The adsorption reached adsorption equilibrium at 2.0h, and the...

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Abstract

The invention discloses a preparation method of ether bond connected multi-carboxyl modified regenerated cellulose. The preparation method comprises the following steps of firstly, converting ester groups of cellulose acetate into hydroxyl groups through saponification reaction; adding halogenated diethyl malonate to carry out base catalysis etherification grafting reaction, enabling the halogen and the hydroxyl groups to carry out grafting reaction, hydrolyzing the ester group of the halogenated diethyl malonate into carboxyl groups, and finally soaking in a dilute acid solution until carboxylate is completely converted into carboxyl groups, so as to obtain an ether bond connected multi-carboxyl modified regenerated cellulose product. According to the method, a multi-carboxyl group is introduced to the surface of the regenerated cellulose through an in-situ etherification reaction, a multi-carboxyl modifier and the regenerated cellulose are firmly bonded and connected through a covalent bond-ether bond, the carboxyl group is not prone to falling off, and a cellulose acetate product cannot be dissolved and swelled along with increase of the number of introduced carboxyl groups, and the product can tolerate a water environment with high pH value, has higher stability and adsorption capacity in the environment, and can be used for removing heavy metal ions.

Description

technical field [0001] The invention belongs to the field of modification of regenerated cellulose, in particular to a preparation method of ether bond-linked multi-carboxyl modified regenerated cellulose. Background technique [0002] With people's attention to the ecological environment, various technical means for water pollution control have developed rapidly. The removal of heavy metal ions in water has always been a research hotspot. Among them, the removal of heavy metal ions by adsorption technology is a simple and effective method. One of the most environmentally friendly methods. Studies have shown that polymer adsorbents have the advantages of high adsorption capacity and good reusability in treating heavy metal polluted wastewater, and biodegradable materials are the first choice for environmentally friendly polymer adsorbents. Among them, cellulose, especially cellulose nanofibers, has outstanding performance in removing heavy metal ions. [0003] It should be...

Claims

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Application Information

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IPC IPC(8): D06M11/38D06M13/21D06M13/144D06M101/08
CPCD06M11/38D06M13/21D06M13/144D06M2101/08Y02P70/62
Inventor 李甫费鹏飞张曼冯宇张志毅刘淑强
Owner TAIYUAN UNIV OF TECH