CN112500502A - Sodium carboxymethylcellulose and preparation method and application thereof - Google Patents
Sodium carboxymethylcellulose and preparation method and application thereof Download PDFInfo
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- 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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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23C13/00—Cream; Cream preparations; Making thereof
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Abstract
The invention relates to the technical field of edible oil and fat, and discloses a preparation method of sodium carboxymethylcellulose and application of the sodium carboxymethylcellulose in production of enzymolysis cream. After the sodium carboxymethyl cellulose is added in the production process of the enzymolysis cream, the high water absorbability of the sodium carboxymethyl cellulose can completely absorb a small amount of water existing after draining, and the water is uniformly dispersed in the enzymolysis cream, so that the water is prevented from being aggregated into liquid drops. The enzymolysis cream produced by the invention can increase the water content from about 0.5 percent to 3.0 to 6.0 percent, and can improve the yield by 2.6 to 5.9 percent. When certain moisture is kept in the enzymolysis cream, the product can be kept moist, smooth and tender, the hardness is reduced, and the use is convenient.
Description
Technical Field
The invention relates to the technical field of edible oil and fat, in particular to a preparation method of sodium carboxymethylcellulose and application of the sodium carboxymethylcellulose in production of enzymolysis cream.
Background
Sodium carboxymethylcellulose is an organic substance, is a carboxymethylated derivative of cellulose, and is the most predominant ionic cellulose gum. Sodium carboxymethylcellulose is an anionic polymer compound usually prepared by reacting natural cellulose with caustic alkali and monochloroacetic acid, and has a molecular weight of several thousands to millions. CMC-Na is white fibrous or granular powder, has no odor, and hygroscopicity, and can be easily dispersed in water to form transparent colloidal solution.
Most of CMC on the market takes ethanol and other organic solvents as reaction media, a reaction kettle is used for production, the crushed cellulose pulp or wood pulp and a reaction reagent are subjected to alkalization etherification reaction, and an ethanol water solution is generally adopted to wash reaction materials. And the CMC on the market has uneven water absorption capacity and water retention capacity, various and complicated varieties and models, high screening difficulty, large workload, time and labor consumption, and is difficult to find suitable products.
Further, in the actual production process of the enzymolysis cream, the anhydrous cream contains less than or equal to 0.1 percent of water, water is added during fat enzymolysis, and part of water is also generated in the enzymolysis reaction process. After the product is finally cooled, the cream is partially solidified to form solid floating on the water surface, and finally the finished product can be obtained after oil-water separation. The solid-liquid separation is difficult to be completely realized in a short time by using a draining mode, a hot air drying mode (enzymolysis cream is easy to melt) cannot be adopted, and a mode combining draining and cold air blowing is commonly used. However, the moisture on the solid-liquid contact surface cannot be completely removed by using the method, the smoothness of the outer surface of the final product is also affected, and the surface of the product is easy to generate water separation after being subjected to temperature fluctuation in the process of storage and transportation. And the prior art does not have research on the use of sodium carboxymethylcellulose in solving the problem of bleeding of enzymatic cream.
Therefore, the problem that needs to be solved by the technical personnel in the field is how to provide a preparation method of sodium carboxymethyl cellulose and use the prepared sodium carboxymethyl cellulose for solving the problem of water bleeding of enzymatic cream.
Disclosure of Invention
The invention aims to provide a method for solving the problem of water separation of enzymatic hydrolysis cream by using sodium carboxymethyl cellulose. The product has no obvious water residue, and the residual water is uniformly dispersed in the cream (the conventional water is insoluble in oil), so that the water content and the yield of the product are improved, the smoothness and the tenderness of the cream can be kept, and the mouthfeel is improved.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation method of sodium carboxymethylcellulose is characterized by comprising the following preparation steps:
(1) adding natural plant cellulose and hydrochloric acid aqueous solution with the mass concentration of 3-8% into a reaction kettle, acidifying and hydrolyzing at 40-70 ℃ and 18-25KPa pressure, and centrifuging at 3200-3600rpm to obtain a filter cake;
(2) putting the filter cake prepared in the step (1) into a monochloroacetic acid aqueous solution with the mass concentration of 55-75%, adding water, reacting under normal pressure, and centrifuging at 3200-3600rpm to obtain the filter cake;
(3) adding the filter cake prepared in the step (2) into 45-55% sodium hydroxide-alcohol solution, adjusting the pH value, and centrifuging at 3200-3600rpm to obtain a filter cake, namely crude sodium carboxymethylcellulose;
(4) continuously washing the crude sodium carboxymethylcellulose prepared in the step (3) by using 75-85% edible alcohol water solution until the chloride content is lower than 0.5%, thus obtaining refined sodium carboxymethylcellulose;
(5) putting the sodium carboxymethylcellulose prepared in the step (4) into a dryer, and drying;
(6) and (4) crushing the dried sodium carboxymethylcellulose prepared in the step (5), controlling the grain diameter of the discharged material to be less than or equal to 75 microns, and detecting the crushed material to be qualified to obtain the sodium carboxymethylcellulose.
Preferably, the weight ratio of the natural plant cellulose, the hydrochloric acid aqueous solution, the water, the monochloroacetic acid aqueous solution, the sodium hydroxide-alcohol solution and the edible alcohol aqueous solution is as follows: 1-2: 6-12: 9-18: 1-1.5: 2.0-3.0: 8-16.
Preferably, the natural plant fiber in the step (1) is purified cotton of GB/T9107-1999 purified cotton, M15 type.
Preferably, the step (3) is carried out by adjusting the pH value to 7 with sodium hydroxide.
Preferably, the step (5) is dried at the temperature of 100 ℃ and 150 ℃ until the moisture is less than or equal to 8 percent.
The invention provides sodium carboxymethyl cellulose, which has the following indexes:
degree of substitution: 1.00-1.05;
brookfield LVT, 2% viscosity at 25 ℃: 150 to 250 cps;
pH：6.5-7.5；
the sieving rate of 200 meshes is more than or equal to 99.5 percent;
the water absorption rate is more than or equal to 300 percent in 10 min;
the light transmittance of the aqueous solution is more than or equal to 99.5 percent;
the water-insoluble impurities are less than or equal to 5 particles/10 g.
The invention provides an application method of sodium carboxymethylcellulose in enzymolysis cream, which comprises the following steps:
(1) melting anhydrous butter in a jacketed kettle at 60-70 deg.C, adding lipase water solution, and performing enzymolysis of butter;
(2) deactivating enzyme and sterilizing the enzymolyzed cream at 90-95 deg.C for 20-25min, cooling to 20-25 deg.C, solidifying the enzymolyzed cream into solid floating on the water;
(3) discharging water from the bottom of the tank to obtain enzymolysis cream;
(4) adding the prepared sodium carboxymethylcellulose into hot water at 70-90 ℃ according to 1.5% -3% of the mass of the hot water, and emulsifying and dissolving for 10-15min by an emulsifying machine to obtain a sodium carboxymethylcellulose solution;
(5) heating the enzymolysis cream obtained in the step (3) to 50-55 ℃ to become liquid, adding the sodium carboxymethyl cellulose solution prepared in the step (4), continuously stirring for 20-30min at 200-300rpm, homogenizing by a homogenizer, cooling to 20-25 ℃ by a tubular heat exchanger, and immediately filling and packaging;
(6) and (3) putting the filled product into a refrigeration house with the temperature of 4-7 ℃ for cooling and solidification to obtain the finished product of the enzymatic hydrolysis cream.
Preferably, the high-pressure homogenization in the step (5) has a first-stage pressure of 10-11KPa and a second-stage pressure of 5-6 KPa.
Through the technical scheme, compared with the prior art, the beneficial effects are as follows:
(1) by adding the special sodium carboxymethylcellulose product disclosed by the invention, after the sodium carboxymethylcellulose product is uniformly dispersed in the enzymatic hydrolysis cream, the sodium carboxymethylcellulose has stronger water absorption and water retention, so that the surface of the enzymatic hydrolysis cream product is smooth and smooth, and no water can be analyzed out.
(2) The enzymolysis cream produced by the invention can increase the water content from about 0.5 percent to 3.0 to 6.0 percent, and can improve the yield by 2.6 to 5.9 percent. The enzymolysis cream keeps certain moisture, can keep the product moist, smooth and tender, reduces the hardness and is convenient to use.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a microscopic view of the enzyme-hydrolyzed cream prepared in example 4, wherein
Represents fatty acid crystals;
represents a sodium carboxymethyl cellulose molecule.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Adding 1 weight part of M15 type purified cotton (GB/T9107-1999 refined cotton) into a reaction kettle, adding 6 weight parts of 5% hydrochloric acid aqueous solution, acidifying and hydrolyzing at 50 ℃ and 18KPa pressure, and centrifuging at 3400rpm to obtain a filter cake;
(2) adding the filter cake prepared in the step (1) into 9 parts by weight of water and 1 part by weight of 65% monochloroacetic acid aqueous solution, reacting at normal pressure, and centrifuging at 3200rpm to prepare a filter cake;
(3) and (3) adding the filter cake prepared in the step (2) into 8 parts by weight of 75% edible alcohol water solution, adjusting the pH value to 7 by using 2.2 parts by weight of 52% sodium hydroxide-alcohol solution, and centrifuging at 3200rpm to obtain the filter cake, namely the crude sodium carboxymethylcellulose.
(4) Continuously washing the crude sodium carboxymethylcellulose prepared in the step (3) by using 75% edible alcohol water solution until the chloride content is lower than 0.5%, thus obtaining refined sodium carboxymethylcellulose;
(5) putting the sodium carboxymethylcellulose refined in the step (4) into a dryer, and drying at 100 ℃ until the water content is less than or equal to 8%;
(6) and (4) crushing the dried sodium carboxymethylcellulose prepared in the step (5), controlling the grain diameter of the discharged material to be less than or equal to 75 microns, and detecting the crushed material to be qualified to obtain the sodium carboxymethylcellulose.
Example 2
(1) Adding 1.5 weight parts of M15 type purified cotton (GB/T9107-1999 refined cotton) into a reaction kettle, adding 9 weight parts of 5% hydrochloric acid aqueous solution, acidifying and hydrolyzing at 60 deg.C and 20KPa pressure, centrifuging at 3500rpm to obtain filter cake;
(2) adding the filter cake prepared in the step (1) into 14 parts by weight of water and 1.2 parts by weight of 70% monochloroacetic acid aqueous solution, reacting at normal pressure, and centrifuging at 3500rpm to prepare a filter cake;
(3) and (3) adding the filter cake prepared in the step (2) into 12 parts by weight of 80% edible alcohol aqueous solution, adjusting the pH value to 7 by using 2.5 parts by weight of 52% sodium hydroxide-alcohol solution, and centrifuging at 3500rpm to obtain the filter cake, namely the crude sodium carboxymethylcellulose.
(4) Continuously washing the crude sodium carboxymethylcellulose prepared in the step (3) by using 80% edible alcohol water solution until the chloride content is lower than 0.5%, thus obtaining refined sodium carboxymethylcellulose;
(5) putting the sodium carboxymethylcellulose refined in the step (4) into a dryer, and drying at 105 ℃ until the water content is less than or equal to 8%;
(6) and (4) crushing the dried sodium carboxymethylcellulose prepared in the step (5), controlling the grain diameter of the discharged material to be less than or equal to 75 microns, and detecting the crushed material to be qualified to obtain the sodium carboxymethylcellulose.
Example 3
(1) Adding 2 parts by weight of M15 type purified cotton (GB/T9107-type 1999 purified cotton) into a reaction kettle, adding 12 parts by weight of 5% hydrochloric acid aqueous solution, acidifying and hydrolyzing at 70 ℃ and 23KPa pressure, and centrifuging at 3600rpm to obtain a filter cake;
(2) adding the filter cake prepared in the step (1) into 18 parts by weight of water and 1.5 parts by weight of 75% monochloroacetic acid aqueous solution, reacting at normal pressure, and centrifuging at 3600rpm to prepare a filter cake;
(3) adding the filter cake prepared in the step (2) into 16 parts by weight of 85% edible alcohol water solution, adjusting the pH value to 7 by using 3.0 parts by weight of 50% sodium hydroxide-alcohol solution, and centrifuging at 3600rpm to obtain the filter cake, namely the crude sodium carboxymethylcellulose.
(4) Continuously washing the crude sodium carboxymethylcellulose prepared in the step (3) by using 85% edible alcohol water solution until the chloride content is lower than 0.5%, thus obtaining refined sodium carboxymethylcellulose;
(5) putting the sodium carboxymethylcellulose refined in the step (4) into a dryer, and drying at 110 ℃ until the water content is less than or equal to 8%;
(6) and (4) crushing the dried sodium carboxymethylcellulose prepared in the step (5), controlling the grain diameter of the discharged material to be less than or equal to 75 microns, and detecting the crushed material to be qualified to obtain the sodium carboxymethylcellulose.
Application example 1
The sodium carboxymethylcellulose prepared in examples 1-3 was tested as shown in Table 1:
TABLE 1
From the above detection results, it can be seen that the sodium carboxymethylcellulose prepared in examples 1 to 3 all meet the performance index for solving the bleeding of the enzymatic cream, and the sodium carboxymethylcellulose prepared in example 2 is used for solving the bleeding of the enzymatic cream:
(1) melting anhydrous butter in a jacketed kettle at 66 deg.C, adding lipase water solution, and performing enzymolysis on fatty acid;
(2) after enzyme deactivation and sterilization are carried out on the enzymolyzed cream at the high temperature of 91 ℃ for 20min, the cream is cooled to the room temperature, and the enzymolyzed cream is solidified into solid floating on the water;
(3) discharging water from the bottom of the tank to obtain enzymolysis cream;
(4) adding the sodium carboxymethylcellulose prepared in the example 2 into hot water at 82.0 ℃ according to 2.0% of the mass of the hot water, and emulsifying and dissolving the sodium carboxymethylcellulose in an emulsifying machine for 10min to prepare a sodium carboxymethylcellulose solution;
(5) heating the enzymolysis cream obtained in the step (3) to 53 ℃ to be liquid, adding 4.0% of the sodium carboxymethyl cellulose solution prepared in the step (4), continuously stirring (250rpm), homogenizing by a homogenizer (the first-stage pressure is 11.0KPa, the second-stage pressure is 5.2KPa), cooling to 22.5 ℃ by a tubular heat exchanger, and immediately filling and packaging;
(6) and (3) putting the filled product into a refrigeration house with the temperature of 5.2 ℃ for cooling and solidification to obtain the finished product of the enzymolysis cream.
The prepared enzymolysis cream is detected according to GB 5408.1-1999, wherein the water content is measured by Karl Fischer method, and the detection result is as follows:
organization state: smooth, normal tissue state and no water immersion on the surface;
color: normal, uniform and consistent;
and (3) flavor nourishing: has strong cream fragrance and no other peculiar smell;
water content: 5.1 percent.
According to the application examples, the invention provides the method for solving the problem of bleeding of the enzymatic cream by using the sodium carboxymethyl cellulose, the method can ensure that the product has no obvious moisture residue, and the residual moisture is uniformly dispersed in the cream (the conventional water is insoluble in oil), so that the moisture content and the yield of the product are improved, the smoothness and the tenderness of the cream can be kept, and the mouthfeel is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The preparation method of sodium carboxymethylcellulose is characterized by comprising the following preparation steps:
(1) adding natural plant cellulose and hydrochloric acid aqueous solution with the mass concentration of 3-8% into a reaction kettle, acidifying and hydrolyzing at 40-70 ℃ and 18-25KPa pressure, and centrifuging at 3200-3600rpm to obtain a filter cake;
(2) putting the filter cake prepared in the step (1) into a monochloroacetic acid aqueous solution with the mass concentration of 55-75%, adding water, reacting under normal pressure, and centrifuging at 3200-3600rpm to obtain the filter cake;
(3) adding the filter cake prepared in the step (2) into a sodium hydroxide-alcohol solution with the mass concentration of 45-55%, adjusting the pH value, and centrifuging at 3200-3600rpm to obtain the filter cake, namely the crude sodium carboxymethylcellulose;
(4) continuously washing the crude sodium carboxymethylcellulose prepared in the step (3) by using 75-85% edible alcohol water solution until the chloride content is lower than 0.5%, thus obtaining refined sodium carboxymethylcellulose;
(5) putting the sodium carboxymethylcellulose prepared in the step (4) into a dryer, and drying;
(6) and (4) crushing the dried sodium carboxymethylcellulose prepared in the step (5), controlling the grain diameter of the discharged material to be less than or equal to 75 microns, and detecting the crushed material to be qualified to obtain the sodium carboxymethylcellulose.
2. The method for preparing sodium carboxymethylcellulose according to claim 1, wherein the weight ratio of the natural plant cellulose, the hydrochloric acid aqueous solution, the water, the monochloroacetic acid aqueous solution, the sodium hydroxide-alcohol solution and the edible alcohol aqueous solution is as follows: 1-2: 6-12: 9-18: 1-1.5: 2.0-3.0: 8-16.
3. The method for preparing sodium carboxymethylcellulose according to claim 1, wherein the natural plant fiber of step (1) is purified cotton of GB/T9107-1999 purified cotton, M15 type.
4. The method for preparing sodium carboxymethylcellulose according to claim 1, wherein the step (3) is carried out by adjusting the pH value to 7 with sodium hydroxide.
5. The method for preparing sodium carboxymethylcellulose according to claim 1, wherein the drying in step (5) is carried out at 100-150 ℃ until the moisture content is less than or equal to 8%.
6. The sodium carboxymethyl cellulose prepared by the method for preparing sodium carboxymethyl cellulose according to any one of claims 1 to 5, wherein the index of the sodium carboxymethyl cellulose is as follows:
degree of substitution: 1.00-1.05;
brookfield LVT, 2% viscosity at 25 ℃: 150-250 cps;
pH：6.5-7.5；
the sieving rate of 200 meshes is more than or equal to 99.5 percent;
the water absorption rate is more than or equal to 300 percent in 10 min;
the light transmittance of the aqueous solution is more than or equal to 99.5 percent;
the water-insoluble impurities are less than or equal to 5 particles/10 g.
7. The application of the sodium carboxymethylcellulose in the enzymatic hydrolysis cream as claimed in claim 6, which is characterized by comprising the following steps:
(1) melting anhydrous butter in a jacketed kettle at 60-70 deg.C, adding lipase water solution, and performing enzymolysis of butter;
(2) deactivating enzyme and sterilizing the enzymolyzed cream at 90-95 deg.C for 20-25min, cooling to 20-25 deg.C, solidifying the enzymolyzed cream into solid floating on the water;
(3) discharging water from the bottom of the tank to obtain enzymolysis cream;
(4) adding the prepared sodium carboxymethylcellulose into hot water at 70-90 ℃ according to 1.5% -3% of the mass of the hot water, and emulsifying and dissolving for 10-15min by an emulsifying machine to obtain a sodium carboxymethylcellulose solution;
(5) heating the enzymolysis cream obtained in the step (3) to 50-55 ℃ to become liquid, adding the sodium carboxymethyl cellulose solution prepared in the step (4), continuously stirring for 20-30min at 200-300rpm, homogenizing by a homogenizer, cooling to 20-25 ℃ by a tubular heat exchanger, and immediately filling and packaging;
(6) and (3) putting the filled product into a refrigeration house with the temperature of 4-7 ℃ for cooling and solidification to obtain the finished product of the enzymatic hydrolysis cream.
8. The application of sodium carboxymethylcellulose in the enzymatic hydrolysis cream according to claim 7, wherein the primary pressure of the high-pressure homogenization in the step (5) is 10-11KPa, and the secondary pressure is 5-6 KPa.
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Application publication date: 20210316 |