Synthesis method of high-carboxylation-degree oxidized cellulose

A technology for oxidizing cellulose and a synthesis method, which is applied in the field of synthesizing oxidized cellulose, can solve problems such as limiting the application range of oxidized cellulose, achieve high carboxylation degree, improve hydrolysis efficiency, and promote the effect of oxidation process

Inactive Publication Date: 2015-12-09
JIANGSU LANWAN BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the Chinese patent (CN101724078A) uses nitric acid and nitrite or nitrogen dioxide as an oxidant to oxidize cellulose in an inert solution, and the carboxyl content in the final product is 8%-12%; the Chinese patent (CN103864940A) uses An oxidation system containing a hydroxylamine compound catalyst as an oxidizing agent, and using sodium hypochlorite or oxygen as an oxidizing agent to oxidize the cellulose material, the carboxyl content of the final product obtained is 1.1%-5.6%; however, the low carboxyl content limits the application of oxidized cellulose For example, if oxidized cellulose is made into medical absorbable hemostatic gauze, the carboxyl content in the cellulose needs to be more than 18%; if oxidized cellulose is used as an anticoagulant, a higher carboxyl content is required

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing treatment, then put the crushed refined cotton and 60g of dry ice into a ball mill jar, seal the device and perform ball milling at 400rmp speed for 3 days ; Open the sealed cover after ball milling, expose the sample to the air and emit bright light, and obtain the pretreated cellulose material;

[0022] Step 2: Multi-step oxidation process of cellulosic material: Take 10 g of pretreated cellulosic material into a container, add 10 g of NaNO 3 , put the beaker in an ice bath, and slowly add 150 mL of 15% H 2 SO 4 , stirred for 1h to obtain mixture 1; slowly add 10gKClO to mixture 1 4 , the reaction temperature was set at 30°C, the oxidation reaction time was 30min, and mixture 2 was obtained; then 15g KClO was added to mixture 2, and then 400mL of deionized water was added, the reaction temperature was set at 50°C, and the reaction time of stirring was 50min, and mixture 3 was obtain...

Embodiment 2

[0025] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing treatment, then put the crushed refined cotton and 80g of dry ice into a ball mill jar, seal the device and perform ball milling at a speed of 600rmp for 2 days ; Open the sealed cover after ball milling, expose the sample to the air and emit bright light, and obtain the pretreated cellulose material;

[0026] Step 2: Multi-step oxidation process of cellulosic material: Take 10g of pretreated cellulosic material into a container, add 12g NaNO 3 , put the beaker in an ice bath, and slowly add 200 mL of 20% H 2 SO 4 , stirred for 1.5h to obtain mixture one; slowly add 15gKClO to mixture one 4 , the reaction temperature is set to 35°C, the oxidation reaction time is 40min, and the mixture 2 is obtained; then 20g KClO is added to the beaker of the mixture 2, and then 500mL deionized water is added, the reaction temperature is set to 55°C, and the stirring reaction time is 55min, and the m...

Embodiment 3

[0029] Step 1: Pretreatment of cellulose material: Weigh 20g of refined cotton for crushing, then put the crushed refined cotton and 90g of dry ice into a ball mill jar, seal the device and rotate it at 800rmp for 2 days ; After ball milling, open the sealed cover, expose the sample to the air and emit bright light, and obtain the pretreated sample;

[0030] Step 2: Multi-step oxidation process of cellulosic material: Take 10 g of pretreated cellulosic material into a container, add 15 g of NaNO 3 , put the beaker in an ice bath, and slowly add 250 mL of 25% H 2 SO 4 , stirred for 2h to obtain mixture one; slowly add 25gKClO to mixture one 4, the reaction temperature was set at 35°C, the oxidation reaction time was 50min, and mixture 2 was obtained; then 30g KClO was added to mixture 2, and then 700mL of deionized water was added, the reaction temperature was set at 55°C, and the stirring reaction time was 60min, and mixture 3 was obtained ;

[0031] Step 3: Subsequent pro...

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Abstract

The invention discloses a synthesis method of high-carboxylation-degree oxidized cellulose, comprising the steps of combining pre-treatment and multistep oxidization to fully oxidize a cellulosic material, namely, first sealing, mixing and ball-milling the cellulosic material and dry ice and exposing a sample to air to realize the pre-treatment process after finishing ball-milling, then adopting NaNO3 and H2SO4 for carrying out primary oxidization on the material, and carrying out secondary oxidization by adopting KCLO4 as an oxidizing agent, wherein a reaction is performed at the temperature of 30 to 40 DEG C and the reaction time is 30 to 60 min; finally, further oxidizing the material subjected to the secondary oxidization by adopting KCLO, wherein the oxidization temperature is 50 to 60 DEG C and the time is 50 to 65 min. An oxidized cellulose product obtained through the synthesis method is relatively high in content of carboxyl, the content of the carboxyl can reach up to 35.6 percent to 48.7 percent, and the product has good application prospect in the technical field of biological medicine materials.

Description

technical field [0001] The invention relates to the technical field of biomedical materials, in particular to a method for synthesizing oxidized cellulose with a high degree of carboxylation. Background technique [0002] Cellulose is a linear semi-rigid natural polymer compound formed by D-glucopyranose anhydrous and β-1,4-glycosidic bonds. There are 3 active hydroxyl groups on each glucosyl ring in its macromolecular chain ( Two secondary hydroxyl groups and one primary hydroxyl group), generally speaking, the oxidation reactions of various forms of cellulose mostly occur on these three hydroxyl groups, which can form aldehyde groups, ketone groups and carboxyl groups. As a polyhydroxy compound, cellulose is easily oxidized by oxidants, and different hydroxyl groups can undergo different oxidation reactions. There are mainly the following possible oxidation methods: ① The primary hydroxyl group is oxidized to an aldehyde group, and can continue to be oxidized to a carboxyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/04
Inventor 章祥庆唐海健
Owner JIANGSU LANWAN BIOTECH
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