CN105713098A - Method for preparing sodium carboxymethyl cellulose by fermenting bagasse - Google Patents
Method for preparing sodium carboxymethyl cellulose by fermenting bagasse Download PDFInfo
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- CN105713098A CN105713098A CN201610228906.8A CN201610228906A CN105713098A CN 105713098 A CN105713098 A CN 105713098A CN 201610228906 A CN201610228906 A CN 201610228906A CN 105713098 A CN105713098 A CN 105713098A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B11/00—Preparation of cellulose ethers
- C08B11/02—Alkyl or cycloalkyl ethers
- C08B11/04—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals
- C08B11/10—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals
- C08B11/12—Alkyl or cycloalkyl ethers with substituted hydrocarbon radicals substituted with acid radicals substituted with carboxylic radicals, e.g. carboxymethylcellulose [CMC]
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a method for preparing sodium carboxymethyl cellulose by fermenting bagasse and belongs to the technical field of preparation of sodium carboxymethyl cellulose. According to the method, waste bagasse is collected, ground and subjected to mixed fermentation with deionized water, a fermented product is subjected to roasting, washing and vacuum freeze drying, a dried product is mixed with glacial acetic acid, sodium hydroxide and the like for modification, a modified product is mixed with a sodium hydroxide solution and heated in a water bath, pH is regulated, a product is mixed with absolute ethyl alcohol and subjected to ultrasonic dispersion, a filter cake is obtained through pumping filtration and mixed with hydrochloric acid, pH is regulated with the sodium hydroxide solution, centrifugation is performed, a supernatant is collected, concentrated, washed and dried, and sodium carboxymethyl cellulose is prepared. The method has the beneficial effects as follows: the preparation steps are simple, the etherification efficiency of a product is increased by 24.3% or more, the product quality is uniform, the viscosity of the product is increased by 18%-23%, and the substitution uniformity is good.
Description
Technical field
The present invention relates to a kind of method that sodium carboxymethyl cellulose prepared by bagasse that ferments, belong to sodium carboxymethyl cellulose preparing technical field.
Background technology
Sodium carboxymethyl cellulose, is called for short CMC, is cellulosic carboxyl methylation derivant, has another name called cellulose gum, be topmost ionic cellulose element glue.In recent years, the CMC of different qualities is used in the different field of industry and people's life, is widely used in the industries such as oil, chemical industry, detergent, pottery, Medicated cigarette, printing and dyeing, weaving, food, medicine, welding rod, has the title of " industry monosodium glutamate ".The purposes of CMC widely, nontoxic, corrosion-free, harmless, free from environmental pollution, cohesive force by force, do not go mouldy, insect-free, can as emulsifying agent, thickening agent, stabilizer, sizing agent, film former, binding agent etc..The production method of CMC mainly has: hydrophily method: the reaction carried out when being and alkali cellulose and etherifying agent are existed free alkali and water.The equipment that is characterized in is simple, small investment, cost are low, but product quality is uneven, ether effect is low, and the viscosity producing product is low.Solvent method: also known as organic solvent method, be exist carry out when organic solvent makes reaction medium alkalizing, the process of etherification reaction, be divided into again slurry process and kneading method according to the number of reaction diluent consumption.The feature of the method be course of reaction heat transfer, mass transfer rapidly, uniformly；Primary response speed is fast, and side reaction is few, and etherifying agent utilization ratio relatively water coal method is high by 10～20%；Reaction stability, replaces uniform poor performance, and organic solvent consumption is big, and equipment investment is big, and production cost is high.
Summary of the invention
The technical problem to be solved: the sodium carboxymethyl cellulose product quality prepared for current method is uneven, ether effect is low, the viscosity producing product is low, replace the drawback of uniform poor performance, provide a kind of collection and discard bagasse, size-reduced with deionized water mixed fermentation after, random micropore is formed by mold fermentation, then through roasting, washing, after vacuum lyophilization, with glacial acetic acid, sodium hydroxide etc. are mixed and modified, again with sodium hydroxide solution mixing heating in water bath, after regulating pH, with dehydrated alcohol mixing ultrasonic disperse, sucking filtration obtains filter cake, with mixed in hydrochloric acid, pH is regulated with sodium hydroxide solution, it is performing centrifugal separation on, collect supernatant, concentrated, washing, the dry method preparing sodium carboxymethyl cellulose.Preparation process of the present invention is simple, and products obtained therefrom ether effect and viscosity are high, replace uniform performance good.
For solving above-mentioned technical problem, the present invention adopts the technical scheme as described below to be:
(1) collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 25～30 DEG C of lower seals fermentations 5～7 days；
(2) after fermentation to be sealed completes, it is placed at 85～100 DEG C and roasts 3～5min, again with after deionized water wash 3～5 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 35～55 parts of dry fermentation bagasse fibres, 30～35 parts of glacial acetic acid, 10～15 parts of sodium hydroxide and 5～15 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 10～15min, is prepared into using modified bagasse fiber；
(3) 1:1 in mass ratio, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 1～2h at 70～80 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 10～15min, after being added dropwise to complete, is placed under 200～300W ultrasonic disperse 10～15min to its stirring mixing；
(4) after ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 10～15min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.3～8.5, stirring mixing is placed under 7500～8800r/min centrifugation 10～15min；
(5) after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 85～90 DEG C, collect crystal and with absolute ethanol washing 2～3 times, then at 65～80 DEG C, dry 6～8h, sodium carboxymethyl cellulose can be prepared into.
The sodium carboxymethyl cellulose degree of polymerization 230～512 that the present invention prepares, molecular weight is 23000～50500, and average actual substitution value is 0.62～1.45, and 1% solution viscosity values is 500～10000mPa.s, keeps one week viscosity unchanged at 28～30 DEG C.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and products obtained therefrom ether effect improves more than 24.3%；
(2) this uniform in quality, the viscosity producing product improves 18～25%, replaces uniform performance good.
Detailed description of the invention
First collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 25～30 DEG C of lower seals fermentations 5～7 days；Then after fermentation to be sealed completes, it is placed at 85～100 DEG C and roasts 3～5min, again with after deionized water wash 3～5 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 35～55 parts of dry fermentation bagasse fibres, 30～35 parts of glacial acetic acid, 10～15 parts of sodium hydroxide and 5～15 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 10～15min, is prepared into using modified bagasse fiber；1:1 in mass ratio again, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 1～2h at 70～80 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 10～15min, after being added dropwise to complete, is placed under 200～300W ultrasonic disperse 10～15min to its stirring mixing；After ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 10～15min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.3～8.5, stirring mixing is placed under 7500～8800r/min centrifugation 10～15min；Finally after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 85～90 DEG C, collect crystal and with absolute ethanol washing 2～3 times, then at 65～80 DEG C, dry 6～8h, sodium carboxymethyl cellulose can be prepared into.
Example 1
First collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 25 DEG C of lower seals fermentations 5 days；Then after fermentation to be sealed completes, it is placed at 85 DEG C and roasts 3min, again with after deionized water wash 3 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 35 parts of dry fermentation bagasse fibres, 35 parts of glacial acetic acid, 15 parts of sodium hydroxide and 15 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 10min, is prepared into using modified bagasse fiber；1:1 in mass ratio again, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 1h at 70 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 10min, after being added dropwise to complete, is placed under 200W ultrasonic disperse 10min to its stirring mixing；After ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 10min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.3, stirring mixing is placed under 7500r/min centrifugation 10min；Finally after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 85 DEG C, collect crystal and with absolute ethanol washing 2 times, then at 65 DEG C, dry 6h, sodium carboxymethyl cellulose can be prepared into.Preparation process of the present invention is simple, and products obtained therefrom ether effect improves 24.5%；This uniform in quality, the viscosity producing product improves 18%, replaces uniform performance good；The sodium carboxymethyl cellulose degree of polymerization 230 prepared, molecular weight is 23000, and average actual substitution value is 0.62, and 1% solution viscosity values is 500mPa.s, keeps one week viscosity unchanged at 28 DEG C.
Example 2
First collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 28 DEG C of lower seals fermentations 6 days；Then after fermentation to be sealed completes, it is placed at 92 DEG C and roasts 4min, again with after deionized water wash 4 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 45 parts of dry fermentation bagasse fibres, 33 parts of glacial acetic acid, 12 parts of sodium hydroxide and 10 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 12min, is prepared into using modified bagasse fiber；1:1 in mass ratio again, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 2h at 75 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 13min, after being added dropwise to complete, is placed under 250W ultrasonic disperse 13min to its stirring mixing；After ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 13min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.4, stirring mixing is placed under 8100r/min centrifugation 13min；Finally after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 88 DEG C, collect crystal and with absolute ethanol washing 3 times, then at 72 DEG C, dry 7h, sodium carboxymethyl cellulose can be prepared into.Preparation process of the present invention is simple, and products obtained therefrom ether effect improves 24.9%；This uniform in quality, the viscosity producing product improves 21%, replaces uniform performance good；The sodium carboxymethyl cellulose degree of polymerization 371 prepared, molecular weight is 36700, and average actual substitution value is 1.03, and 1% solution viscosity values is 5200mPa.s, keeps one week viscosity unchanged at 29 DEG C.
Example 3
First collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 30 DEG C of lower seals fermentations 7 days；Then after fermentation to be sealed completes, it is placed at 100 DEG C and roasts 5min, again with after deionized water wash 5 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 55 parts of dry fermentation bagasse fibres, 30 parts of glacial acetic acid, 10 parts of sodium hydroxide and 5 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 15min, is prepared into using modified bagasse fiber；1:1 in mass ratio again, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 2h at 80 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 15min, after being added dropwise to complete, is placed under 300W ultrasonic disperse 15min to its stirring mixing；After ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 15min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.5, stirring mixing is placed under 8800r/min centrifugation 15min；Finally after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 90 DEG C, collect crystal and with absolute ethanol washing 3 times, then at 80 DEG C, dry 8h, sodium carboxymethyl cellulose can be prepared into.Preparation process of the present invention is simple, and products obtained therefrom ether effect improves 25.2%；This uniform in quality, the viscosity producing product improves 25%, replaces uniform performance good；The sodium carboxymethyl cellulose degree of polymerization 512 prepared, molecular weight is 50500, and average actual substitution value is 1.45, and 1% solution viscosity values is 10000mPa.s, keeps one week viscosity unchanged at 30 DEG C.
Claims (1)
1. the method that sodium carboxymethyl cellulose prepared by the bagasse that ferments, it is characterised in that concrete preparation process is:
(1) collect discarded bagasse, cleaned and dry, pulverize with jet mill subsequently, be prepared into bagasse fibre, in mass ratio 1:1, bagasse fibre is mixed with deionized water and stirring, then be placed on 25～30 DEG C of lower seals fermentations 5～7 days；
(2) after fermentation to be sealed completes, it is placed at 85～100 DEG C and roasts 3～5min, again with after deionized water wash 3～5 times, to its vacuum lyophilization, it is prepared into dry fermentation bagasse fibre, then counts by weight, weigh 35～55 parts of dry fermentation bagasse fibres, 30～35 parts of glacial acetic acid, 10～15 parts of sodium hydroxide and 5～15 parts of deionized waters respectively and be placed in there-necked flask, stirring mixing 10～15min, is prepared into using modified bagasse fiber；
(3) 1:1 in mass ratio, the using modified bagasse fiber of above-mentioned preparation is mixed with the sodium hydroxide solution stirring that mass concentration is 10%, heating in water bath 1～2h at 70～80 DEG C subsequently, after regulating pH to 7.0 with glacial acetic acid again, it is slowly added dropwise the dehydrated alcohol identical with sodium hydroxide solution volume, control time for adding is 10～15min, after being added dropwise to complete, is placed under 200～300W ultrasonic disperse 10～15min to its stirring mixing；
(4) after ultrasonic disperse completes, to its sucking filtration and collect filter cake, 1:5 in mass ratio subsequently, filter cake is mixed 10～15min with the hydrochloric acid stirring that mass concentration is 20%, subsequently its dropping sodium hydroxide solution being regulated pH to 8.3～8.5, stirring mixing is placed under 7500～8800r/min centrifugation 10～15min；
(5) after being centrifuged, collect the supernatant, be placed on rotary evaporated to dryness at 85～90 DEG C, collect crystal and with absolute ethanol washing 2～3 times, then at 65～80 DEG C, dry 6～8h, sodium carboxymethyl cellulose can be prepared into.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107647197A (en) * | 2017-10-31 | 2018-02-02 | 定远县和润水产养殖专业合作社 | A kind of mixed feed for increasing freshwater shrimp premunition |
| CN107691888A (en) * | 2017-10-31 | 2018-02-16 | 定远县和润水产养殖专业合作社 | A kind of balanced freshwater shrimp feed of nutrition |
| CN110616063A (en) * | 2019-09-17 | 2019-12-27 | 攀枝花学院 | Dust suppressant and preparation method thereof |
-
2016
- 2016-04-14 CN CN201610228906.8A patent/CN105713098A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107647197A (en) * | 2017-10-31 | 2018-02-02 | 定远县和润水产养殖专业合作社 | A kind of mixed feed for increasing freshwater shrimp premunition |
| CN107691888A (en) * | 2017-10-31 | 2018-02-16 | 定远县和润水产养殖专业合作社 | A kind of balanced freshwater shrimp feed of nutrition |
| CN110616063A (en) * | 2019-09-17 | 2019-12-27 | 攀枝花学院 | Dust suppressant and preparation method thereof |
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