CN104403007A - Method for preparing sodium carboxymethyl cellulose - Google Patents
Method for preparing sodium carboxymethyl cellulose Download PDFInfo
- Publication number
- CN104403007A CN104403007A CN201410782087.2A CN201410782087A CN104403007A CN 104403007 A CN104403007 A CN 104403007A CN 201410782087 A CN201410782087 A CN 201410782087A CN 104403007 A CN104403007 A CN 104403007A
- Authority
- CN
- China
- Prior art keywords
- mucine
- xylo
- etherification
- method preparing
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention belongs to the field of natural polymer material chemical modification, and relates to a preparation method for high-substitution-degree and high-viscosity sodium carboxymethyl cellulose. The method comprises the following steps: taking and placing dried and smashed cellulose into a hydrothermal reaction kettle, adding an ethanol solution with a certain volume, dropwise adding1-3 ml of a 40% NaOH solution while stirring, and performing alkalization for 1-3 hours at 35 DEG C; after the alkalization is completed, adding sodium chloroacetate with the mass ratio of 1:(0.8-1.6), wherein the etherification temperature is 60-80 DEG C, and the etherification time is 1-3 h; after the reaction is completed, adjusting the pH value to be neutral by using glacial acetic acid, cooling to the room temperature, adding ethyl alcohol with 5 times of volume, stirring and dispersing for 10 min, performing suction filtration, washing with 90% ethyl alcohol for 3 times, finally, washing with ethyl alcohol for one time, and performing vacuum drying, so as to obtain the sodium carboxymethyl cellulose.
Description
Technical field:
The invention belongs to natural macromolecular material field of chemical modification, relate to a kind of preparation method of sodium carboxymethyl cellulose with high degree of substitution and high viscosity.
Background technology:
Mierocrystalline cellulose is a kind of natural high moleculer eompound, the polysaccharide macro-molecular that its chemical structure is is basic ring with anhydrous beta-glucose, and each basic ring has a primary hydroxyl and two secondary hydroxyls.By carrying out chemical modification to it, can obtain a series of cellulosic derivative, namely ether of cellulose is wherein a kind of.Xylo-Mucine (CMC-Na) is a kind of negatively charged ion, straight chain, water-soluble cellulose ether, and outward appearance is white or the wadding fibrous powder of micro-yellow, odorless tasteless, nontoxic.The industries such as medical and health, daily-use chemical industry, papermaking, food, building, material can be widely used in, be commonly called as " industrial monosodium glutamate ".Therefore, the Xylo-Mucine that exploitation high-quality is cheap, for comprehensive utilization renewable resources, exploitation novel material and new technology etc. have positive meaning.
Xylo-Mucine prepared by current domestic application traditional technology not easily disperses in aqueous, and dissolution rate is slow, needs to stir ability dispersing and dissolving for a long time even.Be because cellulosic material gelatinization can form micelle in large water gaging, etherifying reagent is difficult to, deeply to cellulosic crystalline region, cause reaction abundant not, the carboxymethylation product substitution value of gained is low, saltiness is large, product water solution in comparatively strong basicity, thermotolerance and salt tolerance poor.Growing along with economic globalization, the ether of cellulose production industry of China faces huge challenge, and under this background, in the urgent need to seeking, a kind of low-consumption high-efficiency, technique are simple, the method preparing Xylo-Mucine of safety and environmental protection.
Summary of the invention:
The object of the present invention is to provide a kind of method preparing sodium carboxymethyl cellulose with high degree of substitution and high viscosity, the method can low-consumption high-efficiency, safety and environmental protection natural cellulose is prepared into Xylo-Mucine.
In order to realize above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and processing step is: get the Mierocrystalline cellulose after drying and crushing in hydrothermal reaction kettle, add the ethanolic soln of certain volume, under agitation dripping solid-to-liquid ratio is the NaOH solution of 1: 1 ~ 3, and alkalize 1 ~ 3h at 35 DEG C.After alkalization, add the sodium chloroacetate that mass ratio is 1: 0.8 ~ 1.6, etherification temperature is 60 ~ 80 DEG C, and etherification time is 3 ~ 5h, use ice alcohol acid for adjusting pH to neutral after completion of the reaction, be cooled to room temperature, then add 5 times of volume ethanol dispersed with stirring 10min, suction filtration, and by 90% washing with alcohol 3 times, finally with washing with alcohol once, vacuum-drying, obtains Xylo-Mucine.
Beneficial effect of the present invention:
Compared with traditional preparation technology, present invention process route is simple, mild condition, convenient operation, safety and environmental protection, can not only obtain the Xylo-Mucine of high substitution value, and the solvent in preparation process can be recycled, preparation technology's greenization aspect is made to have important meaning.
Embodiment
The present invention adopts 80% ethanolic soln as solvent, and processing step is: get the Mierocrystalline cellulose after drying and crushing in hydrothermal reaction kettle, add the ethanolic soln of certain volume, and under agitation dripping solid-to-liquid ratio is the NaOH solution of 1: 1 ~ 3, and alkalize 1 ~ 3h at 35 DEG C.After alkalization, add the sodium chloroacetate that mass ratio is 1: 0.8 ~ 1.6, etherification temperature is 60 ~ 80 DEG C, and etherification time is 3 ~ 5h, use ice alcohol acid for adjusting pH to neutral after completion of the reaction, be cooled to room temperature, then add 5 times of volume ethanol dispersed with stirring 10min, suction filtration, and by 90% washing with alcohol 3 times, finally with washing with alcohol once, vacuum-drying, obtains Xylo-Mucine.
The present invention selects NaOH consumption, alkalization time, etherifying agent consumption, etherification temperature and etherification time as the influence factor preparing Xylo-Mucine respectively, visible table 1, table 2, table 3, table 4, table 5.
Table 1 NaOH consumption is on the impact preparing Xylo-Mucine
| Sequence number | NaOH/ solid-to-liquid ratio | Alkalization time/h | Etherifying agent/mass ratio | Etherification temperature/DEG C | Etherification time/h | Substitution value |
| 1 | 1∶1 | 1.5h | 1∶1.2 | 65 | 4 | 0.32 |
| 2 | 1∶1.5 | 1.5h | 1∶1.2 | 65 | 4 | 0.56 |
| 3 | 1∶2 | 1.5h | 1∶1.2 | 65 | 4 | 0.7 |
| 4 | 1∶2.5 | 1.5h | 1∶1.2 | 65 | 4 | 0.89 |
| 5 | 1∶3 | 1.5h | 1∶1.2 | 65 | 4 | 0.8 |
Table 2 alkalization time is on the impact preparing Xylo-Mucine
| Sequence number | NaOH/ solid-to-liquid ratio | Alkalization time/h | Etherifying agent/mass ratio | Etherification temperature/DEG C | Etherification time/h | Substitution value |
| 1 | 1∶2.5 | 1h | 1∶1.2 | 65 | 4 | 0.64 |
| 2 | 1∶2.5 | 1.5h | 1∶1.2 | 65 | 4 | 0.79 |
| 3 | 1∶2.5 | 2h | 1∶1.2 | 65 | 4 | 0.8 |
| 4 | 1∶2.5 | 2.5h | 1∶1.2 | 65 | 4 | 0.94 |
| 5 | 1∶2.5 | 3h | 1∶1.2 | 65 | 4 | 0.92 |
Table 3 etherifying agent consumption is on the impact preparing Xylo-Mucine
| Sequence number | NaOH/ solid-to-liquid ratio | Alkalization time/h | Etherifying agent/mass ratio | Etherification temperature/DEG C | Etherification time/h | Substitution value |
| 1 | 1∶2 | 1.5h | 1∶0.8 | 75 | 4 | 0.78 |
| 2 | 1∶2 | 1.5h | 1∶1.0 | 75 | 4 | 0.79 |
| 3 | 1∶2 | 1.5h | 1∶1.2 | 75 | 4 | 0.89 |
| 4 | 1∶2 | 1.5h | 1∶1.4 | 75 | 4 | 0.39 |
| 5 | 1∶2 | 1.5h | 1∶1.6 | 75 | 4 | 0.32 |
Table 4 etherification temperature is on the impact preparing Xylo-Mucine
| Sequence number | NaOH/ solid-to-liquid ratio | Alkalization time/h | Etherifying agent/mass ratio | Etherification temperature/DEG C | Etherification time/h | Substitution value |
| 1 | 1∶2 | 1.5h | 1∶1.2 | 60 | 4 | 0.79 |
| 2 | 1∶2 | 1.5h | 1∶1.2 | 65 | 4 | 1.02 |
| 3 | 1∶2 | 1.5h | 1∶1.2 | 70 | 4 | 0.81 |
| 4 | 1∶2 | 1.5h | 1∶1.2 | 75 | 4 | 0.7 |
| 5 | 1∶2 | 1.5h | 1∶1.2 | 80 | 4 | 0.66 |
Table 5 etherification time is on the impact preparing Xylo-Mucine
| Sequence number | NaOH/ solid-to-liquid ratio | Alkalization time/h | Etherifying agent/mass ratio | Etherification temperature/DEG C | Etherification time/h | Substitution value |
| 1 | 1∶2 | 1.5h | 1∶1.4 | 75 | 3 | 0.53 |
| 2 | 1∶2 | 1.5h | 1∶1.4 | 75 | 3.5 | 0.65 |
| 3 | 1∶2 | 1.5h | 1∶1.4 | 75 | 4 | 0.74 |
| 4 | 1∶2 | 1.5h | 1∶1.4 | 75 | 4.5 | 0.54 |
| 5 | 1∶2 | 1.5h | 1∶1.4 | 75 | 5 | 0.36 |
As a kind of preferred version, processing step of the present invention is: NaOH solid-to-liquid ratio is 1: 2.5, and alkalization time is 2.5h, and etherifying agent mass ratio is 1: 1.2, and etherification temperature is 65 DEG C, and etherification time is 4h.
Claims (8)
1. prepare the method for Xylo-Mucine for one kind, it is characterized in that, comprise the steps: to the invention belongs to natural macromolecular material field of chemical modification, relate to a kind of preparation method of sodium carboxymethyl cellulose with high degree of substitution and high viscosity, method steps is: get the Mierocrystalline cellulose after drying and crushing in hydrothermal reaction kettle, add the ethanolic soln of certain volume, under agitation dripping solid-to-liquid ratio is the NaOH solution of 1: 1 ~ 3, alkalize 1 ~ 3h at 35 DEG C, after alkalization, add the sodium chloroacetate that mass ratio is 1: 0.8 ~ 1.6, etherification temperature is 60 ~ 80 DEG C, etherification time is 3 ~ 5h, use ice alcohol acid for adjusting pH to neutral after completion of the reaction, be cooled to room temperature, then 5 times of volume ethanol dispersed with stirring 10min are added, suction filtration, and by 90% washing with alcohol 3 times, finally with washing with alcohol once, vacuum-drying, obtain Xylo-Mucine.
2. the method preparing Xylo-Mucine according to claim 1, is characterized in that, described in add certain volume ethanolic soln to be solid-to-liquid ratio be 1: 20 80% ethanolic soln.
3. the method preparing Xylo-Mucine according to claim 1, is characterized in that, the NaOH solution of described dropping is 40%.
4. the method preparing Xylo-Mucine according to claim 1, is characterized in that, described what under agitation drip is the 40%NaOH solution of solid-to-liquid ratio 1: 2.5.
5. the method preparing Xylo-Mucine according to claim 1, is characterized in that, the described 2.5h that alkalizes at 35 DEG C.
6. the method preparing Xylo-Mucine according to claim 1, is characterized in that, described in add the sodium chloroacetate that mass ratio is 1: 1.0.
7. the method preparing Xylo-Mucine according to claim 1, is characterized in that, described etherification temperature is 65 DEG C.
8. the method preparing Xylo-Mucine according to claim 1, is characterized in that, described etherification time is 4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410782087.2A CN104403007A (en) | 2014-12-15 | 2014-12-15 | Method for preparing sodium carboxymethyl cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410782087.2A CN104403007A (en) | 2014-12-15 | 2014-12-15 | Method for preparing sodium carboxymethyl cellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104403007A true CN104403007A (en) | 2015-03-11 |
Family
ID=52640681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410782087.2A Pending CN104403007A (en) | 2014-12-15 | 2014-12-15 | Method for preparing sodium carboxymethyl cellulose |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104403007A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105113208A (en) * | 2015-09-29 | 2015-12-02 | 江苏锦宇环境工程有限公司 | Method for preparing composite material special for manufacturing sunscreen clothes |
| CN105330753A (en) * | 2015-11-25 | 2016-02-17 | 泸州北方化学工业有限公司 | Preparation of sodium carboxymethyl cellulose |
| CN108470912A (en) * | 2018-04-12 | 2018-08-31 | 厦门大学 | A kind of preparation method of negative electrode of lithium ion battery using adhesive |
| CN109007513A (en) * | 2018-08-06 | 2018-12-18 | 福建保安康保健食品有限公司 | A kind of brown sugar fructus lycii algae solid beverage |
| CN109007512A (en) * | 2018-08-06 | 2018-12-18 | 福建保安康保健食品有限公司 | A kind of rock sugar fructus arctii algae solid beverage |
| CN112707969A (en) * | 2020-12-28 | 2021-04-27 | 常熟威怡科技有限公司 | Production process of sodium carboxymethylcellulose by self-esterification reaction |
| CN113603083A (en) * | 2021-08-25 | 2021-11-05 | 江苏思峻机械设备有限公司 | Novel efficient modified CMC (carboxy methyl cellulose) water-phase stripping agent and application method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735324A (en) * | 2010-01-13 | 2010-06-16 | 北京理工大学 | Carboxymethyl cellulose nitrate and preparation method thereof |
| CN101768220A (en) * | 2009-11-27 | 2010-07-07 | 北京理工大学 | Method for preparing carboxymethyl cellulose by cotton dropped on the ground |
-
2014
- 2014-12-15 CN CN201410782087.2A patent/CN104403007A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768220A (en) * | 2009-11-27 | 2010-07-07 | 北京理工大学 | Method for preparing carboxymethyl cellulose by cotton dropped on the ground |
| CN101735324A (en) * | 2010-01-13 | 2010-06-16 | 北京理工大学 | Carboxymethyl cellulose nitrate and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105113208A (en) * | 2015-09-29 | 2015-12-02 | 江苏锦宇环境工程有限公司 | Method for preparing composite material special for manufacturing sunscreen clothes |
| CN105330753A (en) * | 2015-11-25 | 2016-02-17 | 泸州北方化学工业有限公司 | Preparation of sodium carboxymethyl cellulose |
| CN105330753B (en) * | 2015-11-25 | 2017-10-17 | 泸州北方化学工业有限公司 | Sodium carboxymethylcellulose preparation method |
| CN108470912A (en) * | 2018-04-12 | 2018-08-31 | 厦门大学 | A kind of preparation method of negative electrode of lithium ion battery using adhesive |
| CN109007513A (en) * | 2018-08-06 | 2018-12-18 | 福建保安康保健食品有限公司 | A kind of brown sugar fructus lycii algae solid beverage |
| CN109007512A (en) * | 2018-08-06 | 2018-12-18 | 福建保安康保健食品有限公司 | A kind of rock sugar fructus arctii algae solid beverage |
| CN112707969A (en) * | 2020-12-28 | 2021-04-27 | 常熟威怡科技有限公司 | Production process of sodium carboxymethylcellulose by self-esterification reaction |
| CN113603083A (en) * | 2021-08-25 | 2021-11-05 | 江苏思峻机械设备有限公司 | Novel efficient modified CMC (carboxy methyl cellulose) water-phase stripping agent and application method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104403007A (en) | Method for preparing sodium carboxymethyl cellulose | |
| CN103755816B (en) | A kind of preparation method of sodium carboxymethylcellulose | |
| CN103539868B (en) | A kind of method of preparing CMC | |
| CN102127170A (en) | Method for preparing cellulose ether by utilizing wood pulp | |
| CN104592400A (en) | Preparation method of microcrystalline cellulose | |
| CN102391381A (en) | Preparation method of cationic hydroxyethyl cellulose ether | |
| CN101830990A (en) | Instant hydroxypropyl methyl cellulose ether and preparation method thereof | |
| CN104831562A (en) | Hydroxypropyl carboxymethyl waxy corn starch acid dye printing paste and preparation method | |
| CN103709264A (en) | Preparation method of carboxymethyl guar gum | |
| CN103319616A (en) | Ethoxyl octenyl succinate tara gum and preparation method thereof | |
| CN103044557B (en) | Preparation method of octenyl succinic acid modified starch ester | |
| CN105777917A (en) | Preparation method of carboxymethyl starch used for reactive dye printing | |
| CN103172754A (en) | Method for preparing carboxymethylcellulose from ionic liquid | |
| CN104844726A (en) | Production technology of magnesium alginate | |
| CN105153325A (en) | Improved production process of carboxymethyl chitosan | |
| CN103193889A (en) | Preparation and separation method of oxidized microcrystalline cellulose | |
| CN104892773A (en) | Preparation method of high-substitution-degree sodium carboxymethylcellulose | |
| CN105693872A (en) | Preparation method of salt-resistant carboxymethyl starch | |
| CN105713098A (en) | Method for preparing sodium carboxymethyl cellulose by fermenting bagasse | |
| CN102276733B (en) | Method for preparing ethyl cellulose with high degree of substitution | |
| CN104804108B (en) | A kind of production technology of hyperviscosity Algin | |
| CN104592404A (en) | Physical oxidative carboxymethyl composite modified starch and preparation method thereof | |
| CN104829739A (en) | Preparation method of low-viscosity cationic guar gum powder | |
| CN106749712B (en) | A kind of method of semidry method preparation carboxymethyl starch | |
| CN103981749A (en) | Method used for preparing microcrystalline cellulose from reed pulp |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150311 |
|
| WD01 | Invention patent application deemed withdrawn after publication |