CN115260319A - Method for preparing carboxymethyl cellulose by derivatization of cellulose in molten salt hydrate - Google Patents
Method for preparing carboxymethyl cellulose by derivatization of cellulose in molten salt hydrate Download PDFInfo
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- 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]
Abstract
The invention discloses a method for preparing carboxymethyl cellulose by derivatization of cellulose in a molten salt hydrate. The method comprises the following steps: firstly, mixing different types of inorganic salts with deionized water according to a certain molar ratio to prepare a composite molten salt hydrate, then adding a certain amount of cellulose to dissolve the cellulose, then adding sodium hydroxide and sodium chloroacetate according to a certain molar ratio to react under certain conditions, after the reaction is finished, adding methanol to precipitate a product, filtering, washing and drying to obtain the carboxymethyl cellulose solid powder. Finally, the degree of substitution of the carboxymethyl cellulose was measured. According to the invention, by adjusting the molar ratio of the inorganic salt to the deionized water, different types of molten salt hydrates are prepared to be used as a reaction medium for preparing the carboxymethyl cellulose by cellulose derivatization, so that the environmental problem caused by using an organic solvent as the reaction medium is avoided, no additional catalyst is required to be added, the reaction condition is mild, the operation steps are continuous, the process is simple, and the consumption cost is low.
Description
Technical Field
The invention belongs to the technical field of biomass resource utilization, and particularly relates to a method for preparing carboxymethyl cellulose by alkalization and etherification reactions by using a composite molten salt hydrate as a reaction medium. The carboxymethyl cellulose prepared by the method can be widely applied to the industrial fields of food, paper making, coating, paint and the like.
Background
Cellulose is an important constituent of woody biomass, which is the most abundant source on earthThe biomass energy can be widely extracted and separated from plants. The simple molecular formula of cellulose is (C)6H10O5)nWherein n is the degree of polymerization, it takes glucose as monomer, it is made up of numerous glucose units, its glucose unit can be as many as 10000, however each glucose monomer has three hydroxy groups, therefore, these three hydroxy groups have important meanings for the synthesis of carboxymethyl cellulose.
Carboxymethyl cellulose is a water-soluble cellulose derivative, the repeating units of which are linked by β -1,4 glycosidic bonds. On a molecular level, the main difference between carboxymethyl cellulose and cellulose is only that some of the anionic carboxyl groups in its structure replace the hydrogen atoms of some of the hydroxyl groups in the fibril structure. Carboxymethyl cellulose was first synthesized in 1918, but its commercial production was first in germany in the 20 th 20 s of the 20 th century. Because of its unique surface properties, excellent mechanical strength, good hydrophilicity, low synthesis cost, etc., carboxymethyl cellulose is widely used in various advanced application fields, such as food, paper making, textile, pharmaceutical, biomedical, biopharmaceutical, wastewater treatment, energy storage, etc. However, carboxymethyl cellulose is applicable to various fields depending on the degree of substitution. For example, carboxymethyl cellulose with a substitution value of 0.5-1.2 is widely applied to the industrial fields of food additives, papermaking pulp, paint, coating, detergents, well drilling and the like, carboxymethyl cellulose with a substitution value of 0.2-1.5 has wide application in the food industry, can be used as milk-flavored beverage, milk product additives and the like, and carboxymethyl cellulose with a substitution value of 0.3-0.4 can be used for manufacturing medical gauze and has an antibacterial effect. Therefore, the preparation of carboxymethyl cellulose with adjustable and controllable substitution value is of great significance.
At present, most of carboxymethyl cellulose prepared by cellulose derivatization adopts alkaline solution, ionic liquid, organic solvent and the like as a cellulose solvent. However, these solvents have certain disadvantages, are easy to corrode equipment, cause environmental pollution and have high solvent cost. It is known that the degree of substitution of carboxymethyl cellulose depends on the reaction temperature, the reaction time, and the amounts of cellulose and alkalizing agent and etherifying agent added, but the degree of substitution is not easily controlled due to a large number of variables. Therefore, the molten salt hydrate developed by the inventor is used as a reaction medium, and the degree of action and the mode of action of the molten salt hydrate are different from those of a cellulose chain in the reaction process, so that the substitution degree of the carboxymethyl cellulose can be regulated and controlled only by the molar ratio of the salt to the water. In addition, the molten salt hydrate is used as a green solvent, has certain unique advantages, inorganic salt is cheap and easy to obtain, the preparation process is simple to operate, other catalysts are not required to be added, and the environment is not polluted.
Chinese patent 201710837709.0 discloses a method for preparing sodium carboxymethylcellulose by treating bamboo powder by an alkali-enzyme coupling technology. Firstly, pretreating bamboo powder by using an alkali solution, then adding a cellulase solution for treatment, and continuously filtering and drying under reduced pressure to obtain the dried bamboo fiber. Adding bamboo fiber into 95% ethanol and 35% sodium hydroxide solution for alkalization, and adding 75% chloroacetic acid ethanol solution for etherification reaction to obtain carboxymethyl cellulose.
Chinese patent 201410321914.8 discloses a method for preparing carboxymethyl cellulose by using sunflower discs as raw materials and water as a solvent. Mixing a certain amount of 2.5% sodium hydroxide solution and crushed sunflower disc powder in a three-neck flask, soaking to fully swell the sunflower disc, dropwise adding the sodium hydroxide solution and sodium chloroacetate solution, reacting at 70 ℃ for 2 hours, and finally washing and drying the product to obtain the carboxymethyl cellulose.
Chinese patent 201510237187.1 discloses a method for preparing sodium carboxymethylcellulose from straws. The method comprises the steps of firstly preparing a composite biocatalyst and a composite reaction catalyst, adding straw cellulose into a kneader, adding sodium hydroxide, chloroacetic acid and the composite reaction catalyst to carry out stirring reaction, washing a product by using 70-85wt% of methanol solution after the reaction is finished, centrifuging and drying to obtain the carboxymethyl cellulose.
Chinese patent 201510837189.4 discloses a preparation method of sodium carboxymethylcellulose. The method comprises the steps of taking refined cotton as a raw material, weighing the refined cotton, putting the weighed refined cotton into a reaction kettle containing a cellulose activator for alkalization, weighing a cellulose etherifying agent solution, adding the cellulose etherifying agent solution into the reaction kettle, reacting for 60-90min at 72-78 ℃, washing with ethanol and drying to obtain the carboxymethyl cellulose.
Jinchen et al, which uses waste disposable paper cups to prepare carboxymethyl cellulose, first treats paper powder with sodium hydroxide solution, then dissolves it with ethanol as solvent, alkalinizes it with sodium hydroxide, then adds chloroacetic acid to etherify, and prepares carboxymethyl cellulose. (Carbohydrate Polymers,2020,237, 116040)
Duraikkannu et al prepared carboxymethyl cellulose using alginate cellulose. Firstly, grinding a seaweed sample into powder, treating cellulose powder by using 17.5 percent sodium hydroxide solution, dissolving the cellulose powder into mixed solution of sodium hydroxide and isopropanol, and adding chloroacetic acid for etherification to prepare carboxymethyl cellulose, wherein the substitution degree is 0.51. (Carbohydrate Polymers,2017,157, 1604-1610)
Although the carboxymethyl cellulose with a certain degree of substitution can be prepared by the methods, the wastes are used as raw materials and play a certain role in resource utilization, the operation process is complex, not only are various catalysts required to be prepared, but also the pretreatment process of the raw materials is complex, and particularly, water or alcohol is used as a reaction medium, so that the cellulose cannot be fully dissolved, and the substitution reaction of cellulose hydroxyl groups is hindered to a certain extent. Therefore, the molten salt hydrate is used as a reaction medium, the substitution degree of the carboxymethyl cellulose is easy to adjust and control by adjusting the molar ratio of the inorganic salt to the water, the operation process is simple, other catalysts are not required to be prepared, the prepared carboxymethyl cellulose has high purity, and the method is environment-friendly, pollution-free and low in cost, and is favorable for promoting the large-scale production of the carboxymethyl cellulose.
Disclosure of Invention
The invention aims to provide a method for preparing carboxymethyl cellulose by derivatizing cellulose in a molten salt hydrate. The technological process includes dissolving molten salt hydrate as reaction medium with certain amount of cellulose, successively adding certain amount of sodium hydroxide and sodium chloroacetate to react, precipitating, washing, filtering and stoving to obtain carboxymethyl cellulose.
In order to achieve the purpose, the invention provides the following technical scheme:
(1) Mixing two inorganic salts and deionized water according to different molar ratios to obtain a composite molten salt hydrate;
(2) Mixing the composite molten salt hydrate obtained in the step (1) with cellulose, and after the cellulose is dissolved, adding sodium hydroxide and sodium chloroacetate to carry out heating and stirring reaction;
(3) And (3) transferring the product obtained in the step (2) into a beaker, adding methanol, precipitating and filtering the product, adding a small amount of deionized water, dropwise adding acetic acid for neutralization, and washing and filtering the product by using ethanol.
(4) Washing the solid precipitate obtained in the step (3) with methanol and ethanol alternately, and drying to obtain carboxymethyl cellulose powder;
(5) Weighing a certain amount of the carboxymethyl cellulose powder in the step (4), acidifying, washing with methanol and ethanol, and drying;
(6) Weighing a certain amount of the solid powder dried in the step (5), adding deionized water, stirring, adding a sodium hydroxide solution, heating, stirring, adding a phenolphthalein indicator, titrating by using a hydrochloric acid solution, and recording titration data.
Further, in the step (1), the two inorganic salts are mixed with the deionized water according to the molar ratio of 1 (1-2) to 4-8.
Further, the molar ratio of the cellulose to the sodium hydroxide and the sodium chloroacetate added in the step (2) is 1.
Further, in the step (3), 70 to 100mL of ethanol was used for washing.
Further, in the step (4), the methanol and the ethanol are alternately washed for 3 to 8 times, and finally dried for 12 hours at the temperature of 55 ℃.
Further, in the case of treating the carboxymethyl cellulose product in the step (5), 1g of dried carboxymethyl cellulose powder is weighed, stirred in ethanol, added with 1mL of hydrochloric acid (2M) to acidify, heated and stirred for 10min, and the solid phase is washed with ethanol 5 times and dried at 100 ℃ for 3h.
Further, step (6) before titration, 100mg of the dried carboxymethyl cellulose powder was weighed out and dissolved in 20mL of deionized water, 6mL of sodium hydroxide solution (0.2M) was added and boiled under heating for 15min. The concentration of hydrochloric acid used during titration was 0.2M, the titration was carried out in three times and the average volume of hydrochloric acid consumed was recorded.
The invention has the advantages that:
1. the invention takes the composite molten salt hydrate as the cellulose solvent, and does not need to add extra catalyst.
2. The molten salt hydrate is used as a cellulose solvent, so that the cellulose can be quickly and efficiently dissolved, and the cellulose derivatization reaction can be favorably carried out.
3. The method comprises the steps of fully dissolving cellulose, adding sodium hydroxide for alkalization, and then adding an etherifying agent sodium chloroacetate for preparing the carboxymethyl cellulose, wherein the reaction process is a homogeneous system, and the reaction contact area can be increased, so that the substitution degree is increased, and the content of the carboxymethyl cellulose is increased.
4. The method realizes simple regulation and control of the substitution degree of the carboxymethyl cellulose by regulating the molar ratio of the salt to the water.
5. The method is simple to operate, uses environment-friendly green solvent, and has low preparation cost.
Drawings
FIG. 1 is a flow chart of the preparation of carboxymethyl cellulose and the determination of the degree of substitution.
Detailed Description
Example 1:
(1) Mixing LiCl and ZnCl2The two inorganic salts and deionized water were mixed to make up 29.7g in a molar ratio of 12-H2O composite molten salt hydrate;
(2) Weighing four parts of 0.30g cellulose, and respectively adding four kinds of LiCl-ZnCl2-H2Dissolving in O composite molten salt hydrate;
(3) And (3) adding 1.85g of sodium hydroxide and 5.39g of sodium chloroacetate into the dissolved cellulose solution in the step (2), and reacting at 85 ℃ for 4 hours.
(4) Transferring the reaction product in the step (3) into a 250mL beaker, adding 70-100mL of methanol to precipitate and filter the carboxymethyl cellulose product, then adding 10mL of water, dropwise adding acetic acid for neutralization, then adding 70-100mL of ethanol for washing, alternately washing for 3 times by the methanol and the ethanol, and finally drying the filtered precipitate in an oven at 55 ℃ for 12 hours to obtain carboxymethyl cellulose solid powder;
(5) Weighing 1g of carboxymethyl cellulose solid powder obtained in the step (4), and stirring in 20mL of ethanol for 5min. It was converted to the acidic form by the addition of 1mL hydrochloric acid (2M). The solution was heated and stirred for 10min. The resulting solution is divided into a liquid phase and a solid phase. The solid phase is washed 5 times with 10mL of ethanol. The final product was washed with methanol, dried at 100 ℃ for 3h and stored in a desiccator.
(7) Weighing 100mg of the solid carboxymethyl cellulose powder obtained in the step (5), dissolving the solid carboxymethyl cellulose powder in 20mL of deionized water, adding 6mL of sodium hydroxide solution (0.2M), heating, stirring, boiling for 15min, cooling to room temperature, dropwise adding 2 drops of phenolphthalein indicator, titrating the solution with hydrochloric acid (0.2M), and recording the volume of the consumed hydrochloric acid.
(8) Under the same operating conditions as in step (7), a blank was formed without addition of solid carboxymethylcellulose powder, at which point the average volume V of hydrochloric acid was consumedo＝5.18mL。
(9) The carboxymethyl group content and the degree of substitution are calculated according to the following two formulae:
(％CM)＝[(Vo-Vn)M×0.059×100](ii)/m; (degree of substitution) =162 ×% CM/[5900- (58 ×% CM)]
Wherein, Vo= number of ml of hydrochloric acid used for titration of blank solution; vn= number of ml of hydrochloric acid used for titration of sample; m = molar hydrochloric acid used; m = sample amount (g).
(10) Obtained by the above steps (1-9) when LiCl: znCl2:H2O =1n=3.59mL, carboxymethyl content 18.72%, degree of substitution 0.63; when LiCl is ZnCl2:H2O =1, 2n=3.17mL, carboxymethyl content 23.73%, degree of substitution 0.85; when LiCl is ZnCl2:H2O =1n=2.81mL, carboxymethyl content 27.98%, degree of substitution 1.06; when LiCl is ZnCl2:H2O =1, 2n=2.59 mL, the carboxymethyl group content was 30.57%, and the degree of substitution was 1.20.
Example 2:
(1) LiCl and ZnBr are mixed2The two inorganic salts and deionized water were mixed to make up 29.7g according to a molar ratio of 12-H2O composite molten salt hydrate;
(2) Weighing four parts of 0.30g cellulose, and respectively adding four kinds of LiCl-ZnBr2-H2Dissolving in O composite molten salt hydrate;
(3) And (3) adding 1.85g of sodium hydroxide and 5.39g of sodium chloroacetate into the dissolved cellulose solution in the step (2), and reacting for 4 hours at 85 ℃.
(4) Transferring the reaction product in the step (3) into a 250mL beaker, adding 70-100mL of methanol to precipitate and filter the carboxymethyl cellulose product, then adding 10mL of water, dropwise adding acetic acid for neutralization, then adding 70-100mL of ethanol for washing, alternately washing for 5 times by methanol and ethanol, and finally drying the filtered precipitate in an oven at 55 ℃ for 12 hours to obtain carboxymethyl cellulose solid powder;
(5) Weighing 1g of carboxymethyl cellulose solid powder obtained in the step (4), and stirring in 20mL of ethanol for 5min. It was converted to the acidic form by the addition of 1mL hydrochloric acid (2M). The solution was heated and stirred for 10min. The resulting solution is divided into a liquid phase and a solid phase. The solid phase is washed 6 times with 10mL of ethanol. The final product was washed with methanol, dried at 100 ℃ for 3h and stored in a desiccator.
(7) Weighing 100mg of the solid carboxymethyl cellulose powder in the step (5), dissolving the solid carboxymethyl cellulose powder in 20mL of deionized water, adding 6mL of sodium hydroxide solution (0.2M), heating, stirring, boiling for 15min, cooling to room temperature, dropwise adding 2 drops of phenolphthalein indicator, titrating the solution with hydrochloric acid (0.2M), and recording the volume of consumed hydrochloric acid.
(8) Under the same operating conditions as in step (7), a blank was formed without adding solid carboxymethylcellulose powder, at which point the average volume V of hydrochloric acid consumedo＝5.18mL。
(9) The carboxymethyl group content and the degree of substitution are calculated according to the following two formulae:
(％CM)＝[(Vo-Vn)M×0.059×100](ii)/m; (substitution)Degree) =162 ×% CM/[5900- (58 ×% CM)]
Wherein, Vo= number of ml of hydrochloric acid used for titration of blank solution; vn= number of ml of hydrochloric acid used for titration of sample; m = molar concentration of hydrochloric acid used; m = sample amount (g).
(10) Obtained by the above steps (1-9) when LiCl: znBr2:H2O =1n=1.81mL, carboxymethyl content 39.73%, degree of substitution 1.79; when LiCl is ZnBr2:H2O =1, 2n=2.96mL, carboxymethyl content 26.22%, degree of substitution 0.97; when LiCl is ZnBr2:H2O =1n=3.21mL, carboxymethyl content 23.30%, degree of substitution 0.83; when LiCl is ZnBr2:H2O =1, 2n=3.68mL, carboxymethyl content 17.74%, degree of substitution is 0.59.
Example 3:
(1) Reacting LiBr and ZnBr2The two inorganic salts and deionized water were mixed to prepare 29.7g in a molar ratio of 12-H2O composite molten salt hydrate;
(2) Weighing four parts of 0.30g of cellulose, and respectively adding four kinds of LiBr-ZnBr2-H2Dissolving in O composite molten salt hydrate;
(3) And (3) adding 1.85g of sodium hydroxide and 5.39g of sodium chloroacetate into the dissolved cellulose solution in the step (2), and reacting for 4 hours at 85 ℃.
(4) Transferring the reaction product in the step (3) into a 250mL beaker, adding 70-100mL of methanol to precipitate and filter the carboxymethyl cellulose product, then adding 10mL of water, dropwise adding acetic acid for neutralization, then adding 70-100mL of ethanol for washing, alternately washing with methanol and ethanol for 7 times, and finally drying the filtered precipitate in an oven at 55 ℃ for 12 hours to obtain carboxymethyl cellulose solid powder;
(5) Weighing 1g of carboxymethyl cellulose solid powder obtained in the step (4), and stirring in 20mL of ethanol for 5min. It is converted to the acidic form by addition of 1mL hydrochloric acid (2M). The solution was heated and stirred for 10min. The resulting solution is divided into a liquid phase and a solid phase. The solid phase is washed 8 times with 10mL of ethanol. The final product was washed with methanol, dried at 100 ℃ for 3h and stored in a desiccator.
(7) Weighing 100mg of the solid carboxymethyl cellulose powder obtained in the step (5), dissolving the solid carboxymethyl cellulose powder in 20mL of deionized water, adding 6mL of sodium hydroxide solution (0.2M), heating, stirring, boiling for 15min, cooling to room temperature, dropwise adding 2 drops of phenolphthalein indicator, titrating the solution with hydrochloric acid (0.2M), and recording the volume of the consumed hydrochloric acid.
(8) Under the same operating conditions as in step (7), a blank was formed without adding solid carboxymethylcellulose powder, at which point the average volume V of hydrochloric acid consumedo＝5.18mL。
(9) The carboxymethyl content and the degree of substitution are calculated according to the following two formulae:
(％CM)＝[(Vo-Vn)M×0.059×100](ii)/m; (degree of substitution) =162 ×% CM/[5900- (58 ×% CM)]
Wherein, Vo= number of ml of hydrochloric acid used for titration of blank solution; vn= number of ml of hydrochloric acid used for titration of sample; m = molar hydrochloric acid used; m = sample amount (g).
(10) Obtained by the above steps (1-9) when LiBr: znBr2:H2O =1n=3.32mL, carboxymethyl content 21.98%, degree of substitution 0.77; when LiBr is ZnBr2:H2O =1, 2n=2.51mL, carboxymethyl content 31.45%, degree of substitution 1.25; when LiBr is ZnBr2:H2O =1, 2n=2.44mL, carboxymethyl content 32.31%, degree of substitution 1.30; when LiBr is ZnBr2:H2O =1n=3.87mL, carboxymethyl content 15.45%, degree of substitution 0.50.
The results of derivatization in molten salt hydrate to prepare carboxymethyl cellulose according to the present invention are shown in table 1.
TABLE 1
Claims (9)
1. A method for preparing carboxymethyl cellulose by derivatizing cellulose in a molten salt hydrate is characterized by comprising the following steps:
(1) Mixing two inorganic salts and deionized water according to a certain molar ratio to obtain a composite molten salt hydrate;
(2) Mixing the composite molten salt hydrate obtained in the step (1) with a certain mass of cellulose, stirring, heating and reacting, adding a certain mass of sodium hydroxide and sodium chloroacetate after the cellulose is completely dissolved, and continuously stirring, heating and reacting;
(3) Transferring the product reacted in the step (2) into a beaker, adding a proper amount of methanol for precipitation, and filtering the precipitate;
(4) Adding a certain amount of deionized water into the solid filtered in the step (3), neutralizing with acetic acid, and washing with ethanol;
(5) Washing the solid washed in the step (4) by using methanol and ethanol alternately, and drying to obtain carboxymethyl cellulose powder;
(6) Weighing a certain amount of the solid powder dried in the step (5), adding hydrochloric acid for acidification, washing a solid phase with methanol and ethanol, filtering, and finally drying;
(7) Weighing a certain amount of the solid powder dried in the step (6), adding deionized water, stirring, adding a sodium hydroxide solution, heating, stirring, adding a phenolphthalein indicator, and titrating by using a hydrochloric acid solution;
(8) And (4) recording the titration result in the step (7) and calculating the carboxymethyl content and the substitution degree of the carboxymethyl cellulose.
2. The method for preparing carboxymethyl by derivatization of cellulose in the complex molten salt hydrate according to claim 1Process for preparing cellulose, characterized in that the two inorganic salts can be ZnCl2、LiCl、ZnBr2And LiBr.
3. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a complex molten salt hydrate according to claim 1, wherein the molar ratio of the two inorganic salts in the complex molten salt hydrate to deionized water is 1 (1-2) to (4-8).
4. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein the molar ratio of the added cellulose to sodium hydroxide and sodium chloroacetate is 1.
5. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein the temperature for derivatization of the cellulose is 85 ℃ and the reaction time is 4 hours.
6. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein the reaction product of the derivatization of the cellulose is alternately washed with methanol and ethanol for 3 to 8 times, and finally dried at 55 ℃ for 12 hours.
7. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein 1g of dried carboxymethyl cellulose powder is weighed and stirred in ethanol, 1mL of hydrochloric acid (2M) is added for acidification, then the mixture is heated and stirred for 10min, and then the solid phase is washed 5 times with ethanol and dried at 100 ℃ for 3h when processing the carboxymethyl cellulose product.
8. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein 100mg of dry carboxymethyl cellulose powder is weighed out and dissolved in 20mL of deionized water before titration, 6mL of sodium hydroxide solution (0.2M) is added and boiling is carried out for 15min under heating.
9. The method for preparing carboxymethyl cellulose by derivatization of cellulose in a composite molten salt hydrate according to claim 1, wherein the concentration of hydrochloric acid used for titration is 0.2M, the titration is performed in three times, and the average volume of hydrochloric acid consumed is recorded.
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