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A two-stage high-pressure homogeneous method for preparing micro-nano cellulose

A micro-nano cellulose, high-pressure homogenization technology, applied in the post-processing of cellulose pulp, fiber raw material processing, pulp property modification and other directions, can solve the problems of easily blocked product size, high pressure, complex process, etc. Effects of homogenization, avoidance of consumption and contamination, simple preparation process

Active Publication Date: 2019-05-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the homogenization treatment used in the above-mentioned existing patented technologies is mostly one-stage high-pressure homogenization, which has disadvantages such as high pressure, easy blockage in the homogenization process, and uneven product size; some patents are prepared by purely physical methods, and the process is complicated. It has high requirements on equipment and high energy consumption; there is also a patented technology to prepare micro-nano cellulose with low crystallinity, which is inconsistent with the current market demand for products with high crystallinity or certain crystallinity

Method used

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  • A two-stage high-pressure homogeneous method for preparing micro-nano cellulose
  • A two-stage high-pressure homogeneous method for preparing micro-nano cellulose
  • A two-stage high-pressure homogeneous method for preparing micro-nano cellulose

Examples

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Effect test

Embodiment 1

[0041] (1) 50g wood pulp is mixed with 750g mass concentration of 15% dilute sulfuric acid solution to obtain a cellulose suspension, which is centrifugally washed with distilled water after standing for 4h;

[0042] (2) Add 1.5g maleic anhydride to the cellulose processed in step (1), carry out high-pressure homogenization at 8°C, and the pressure is 60MPa; put it into a freeze dryer, and freeze-dry it at -10°C to obtain micro Nanocellulose crystals;

[0043] (3) After the obtained micro-nano cellulose crystals were pretreated for 2 hours at 120° C. and 0.1 MPa, they were taken out, stirred evenly, and placed in an ultrasonic cell pulverizer for ultrasonic treatment for 15 minutes;

[0044] (4) The micro-nano cellulose processed in step (3) is subjected to high-pressure homogenization at a low temperature of 8°C, and the pressure is 80MPa; after homogenization, it is placed in a freeze dryer, and freeze-dried at -10°C to obtain micronanocellulose Nanocellulose.

[0045] The...

Embodiment 2

[0047] (1) 50g waste paper pulp is mixed with 1000g mass concentration of 22% dilute sulfuric acid solution to obtain a cellulose suspension, which is centrifuged and washed with distilled water after standing for 3 hours;

[0048] (2) Add 2.0g maleic anhydride to the cellulose processed in step (1), carry out high-pressure homogenization at 12°C, and the pressure is 65MPa; put it into a freeze dryer, and freeze-dry it at -25°C to obtain micro Nanocellulose crystals;

[0049] (3) After the obtained micro-nano cellulose crystals were pretreated for 2 hours at 121° C. and 0.2 MPa, they were taken out, stirred evenly, and put into an ultrasonic cell pulverizer for ultrasonic treatment for 18 minutes;

[0050] (4) The micro-nano cellulose processed in step (3) is subjected to high-pressure homogenization at a low temperature of 15° C., and the pressure is 100 MPa; after the homogenization treatment, it is placed in a freeze dryer and freeze-dried at -40° C. to obtain micro-nano ce...

Embodiment 3

[0053](1) 40g cotton pulp is mixed with 1000g mass concentration of 35% dilute hydrochloric acid solution to obtain a cellulose suspension, which is centrifugally washed with distilled water after standing for 2.5h;

[0054] (2) Add 2.0g maleic anhydride to the cellulose processed in step (1), carry out high-pressure homogenization at 15°C, and the pressure is 80MPa; put it into a freeze dryer, and freeze-dry it at -40°C to obtain micro Nanocellulose crystals;

[0055] (3) After the obtained micro-nanocellulose crystals were pretreated for swelling at 123°C and 0.3 MPa for 3 hours, they were taken out, stirred evenly, and placed in an ultrasonic cell pulverizer for ultrasonic treatment for 20 minutes;

[0056] (4) The micro-nano cellulose processed in step (3) is subjected to high-pressure homogenization at a low temperature of 12° C., and the pressure is 85 MPa; after the homogenization treatment, it is placed in a freeze dryer and freeze-dried at -20° C. to obtain micro-nano...

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Abstract

The invention discloses a method for preparing micro-nano cellulose by virtue of second-stage high-pressure homogenization. The method comprises the following steps of: (1) mixing a cellulose raw material with a dilute acid solution to obtain cellulose suspension liquid, standing, and carrying out centrifugal washing with water; (2) adding a dispersing agent, and carrying out low-temperature high-pressure homogenization and freeze drying, so as to obtain micro-nano cellulose crystals; (3) carrying out wet expansion on the micro-nano cellulose crystals, taking out, uniformly stirring, putting the crystals into an ultrasonic cell disruptor, and carrying out ultrasonic treatment; and (4) carrying out low-temperature high-pressure homogenization and freeze drying on the micro-nano cellulose after the ultrasonic treatment. By carrying out dilute acid pretreatment, ultrasonic assisting and low-temperature second-stage high-pressure homogenization, the agglomeration of materials caused due to the over-high temperature after the homogenization is prevented, fibers can be uniformly dispersed, and the lengths of the celluloses are not severely damaged, so that the problems that the pressure is high, the blockage easily occurs, the product dimensions are not uniform, and the like in the first-stage mechanical high-pressure homogenization process are effectively solved.

Description

technical field [0001] The invention belongs to the field of plant fiber materials, and in particular relates to the preparation of micro-nano cellulose. Background technique [0002] Plant cellulose is one of the most abundant natural polymer materials in nature. Due to its renewability and non-polluting properties, it has received more and more attention. After plant cellulose is prepared into micro-nano cellulose, it has the basic structure and properties of plant cellulose, and also has the characteristics of micro-nano cellulose itself, such as large specific surface area, super strong adsorption capacity and high strength. [0003] At present, there are mechanical methods, chemical methods, and biological methods to prepare plant micro-nanocellulose. The document with the patent number 2010102139025 discloses a method for preparing nanocellulose fibers by combining ultrasonic treatment with high-pressure homogeneous treatment. Through ultrasonic treatment, the problem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D21C9/00
CPCD21C9/007
Inventor 陈克复曾劲松王斌李金鹏
Owner SOUTH CHINA UNIV OF TECH
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