CN110044845B - Method for measuring content of hemicellulose in xylo-oligosaccharide produced by using viscose waste water - Google Patents
Method for measuring content of hemicellulose in xylo-oligosaccharide produced by using viscose waste water Download PDFInfo
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Abstract
The invention belongs to the technical field of xylo-oligosaccharide production, and provides a method for measuring the content of hemicellulose in xylo-oligosaccharide produced by viscose wastewater. The method comprises the following steps: 1) establishing a standard curve to obtain a linear regression equation Y ═ aX + b; 2) sampling sample liquid; 3) and detecting the sample liquid to finally obtain the content of the detected hemicellulose. According to the method, hemicellulose is dissolved under an alkaline condition, a reducing sugar solid is generated, and the content of the reducing sugar solid is detected by a refraction method, so that the content of the hemicellulose is obtained; the invention has the advantages of high detection accuracy, short period, convenient operation and low cost.
Description
Technical Field
The invention belongs to the technical field of xylo-oligosaccharide production, and particularly relates to a method for measuring the content of hemicellulose in xylo-oligosaccharide produced by viscose wastewater.
Background
Since this century, with the continuous progress of technology, the level of production technology of viscose fiber production enterprises has been significantly improved, and energy-saving and emission-reduction works have also been colored greatly, but still remain a great emission pollution source in the water pollution system of our country in terms of its pollution emission. In the production process of viscose fiber with chemical pulp (wood pulp, cotton pulp, straw pulp, reed pulp and other plant cellulose) as raw material, the first step of producing viscose fiber is to treat (soak, squeeze) cellulose with alkali liquor. The high concentration of hemicellulose has an extremely adverse effect on the production of viscose fibres and on the quality of the finished products, and therefore the hemicellulose must be dissolved out with an alkaline solution in the impregnation process in order to obtain high-strength cellulose. In the above process, a large amount of hemicellulose-rich high-concentration alkaline press liquor, in which sodium hydroxide and hemicellulose are main components, is produced.
The existing method for treating squeezed alkali liquor mostly adopts a nanofiltration technology to separate sodium hydroxide from the sodium hydroxide to obtain pure alkali liquor which can be directly reused in the process, but hemicellulose in trapped liquid still contains partial sodium hydroxide in hemicellulose concentrated solution obtained after concentration, and at present, partial feed liquid is discharged into wastewater for treatment.
Nowadays, viscose waste water after alkali removal is used as a raw material, xylo-oligosaccharide is produced through hemicellulose in the raw material, and the hemicellulose is recycled. However, in the production process of xylo-oligosaccharide, the content of hemicellulose in the raw material needs to be mastered so as to accurately calculate the addition of xylanase for production control, and a method capable of rapidly measuring the content of hemicellulose in the raw material is further needed.
At present, the adopted method for detecting the content of hemicellulose in the raw material is generally a potassium dichromate-redox method, namely: the method comprises the following steps of completely oxidizing hemicellulose by using an excessive potassium dichromate solution, titrating the excessive potassium dichromate by using ammonium ferrous sulfate, and obtaining the content of the hemicellulose according to the consumption of the potassium dichromate, wherein the specific technical scheme comprises the following steps:
firstly, sucking 5mL of a hemicellulose solution sample into a 500mL triangular flask by using a pipette;
secondly, sucking a certain amount of 1mol/L K2Cr2O7Adding standard solution (the addition amount is determined according to the content of hemicellulose) into a triangular flask containing a collected sample, shaking uniformly, and rapidly and accurately adding 20mL of 98% H2SO4Boiling the solution;
and thirdly, standing to cool the solution to room temperature, adding about 150mL of cold desalted water, titrating the solution by using a 0.5 mol/L ammonium ferrous sulfate standard solution, dripping 4-6 drops of a prepared vanadium reagent when the end point is reached, and titrating the solution until the solution is changed from gray black to clear dark green, namely the end point. Recording the consumption of FeSO4·(NH4)2SO4Milliliters of standard solution;
fourthly, making a blank test and calibrating FeSO4·(NH4)2SO4The concentration of (3) is the same as that of the second step and the third step;
and fifthly, calculating the content of hemicellulose.
However, the method has long detection time, high safety risk of adding 98% concentrated sulfuric acid in the detection process, large influence of temperature change on the detection result in the oxidation process and large detection data error.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for measuring the content of hemicellulose in xylo-oligosaccharide produced by viscose wastewater; the method comprises the steps of taking viscose waste water after alkali removal as a raw material, wherein the raw material contains a large amount of hemicellulose and a small amount of sodium hydroxide, detecting the content of solid reducing sugar by a refraction method according to the principle that the hemicellulose is dissolved into solid reducing sugar under an alkaline condition, establishing a standard curve, calculating the relation between the content of the solid reducing sugar and the content of the hemicellulose by using a linear regression equation, finally calculating the content of the hemicellulose in a xylo-oligosaccharide raw material by using the linear regression equation, accurately calculating the addition of xylanase, and controlling the production process of the xylo-oligosaccharide; the invention has the advantages of high detection accuracy, short period, convenient operation and low cost.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a method for measuring the content of hemicellulose in xylo-oligosaccharide produced by viscose wastewater comprises the following steps:
1) establishing a standard curve: s1 preparation: weighing hemicellulose, adding the hemicellulose into distilled water, and stirring until the hemicellulose is completely dissolved to obtain a standard substance with the concentration of 100-200 g/L; then diluting the standard substance into at least 5 standard solutions with different concentrations, then respectively taking the same amount of standard solution, respectively adding the same amount of alkali liquor according to the volume ratio of 1:5 to the standard solution, and standing for 5-10 min; s2 measurement: respectively detecting the content of solid reducing sugar generated in the standard solution by using a refractometer, and recording data; s3, linear regression equation: establishing a standard curve by adopting a unary linear regression method according to the data recorded in the step S2 to obtain a linear regression equation Y ═ aX + b, wherein Y represents the solid content of reducing sugar, and X represents the content of hemicellulose;
2) sampling sample liquid: taking a sample liquid containing hemicellulose with unknown content;
3) and (3) sample liquid detection: x1 pretreatment: adding alkali liquor into the sample solution according to the volume ratio of 1:5 to the sample solution, and standing for 5-10 min; x2 measurement: detecting the content of solid reducing sugar generated in the sample liquid by using a refractometer, and recording data; x3: repeating the step X2 for 2-5 times, and recording data;
4) calculating the content of hemicellulose in the sample liquid: y1: obtaining the average value of the solid content of reducing sugar, namely the Y value according to the data of X2 and X3; y2: and (4) according to the linear regression equation in the step S3, substituting the Y value and calculating the content of the hemicellulose in the sample liquid, namely the X value.
Further, in a preferred embodiment of the present invention, in step S1, the hemicellulose is experimentally pure.
Further, in a preferred embodiment of the present invention, in step 2), the sample solution is a retentate obtained by recovering sodium hydroxide from the viscose waste water, wherein the concentration of hemicellulose in the retentate is 90-110g/L, and the concentration of sodium hydroxide is 40-45 g/L.
Further, in a preferred embodiment of the present invention, the volume of the standard solution is equal to the volume of the sample solution.
Further, in the preferred embodiment of the present invention, the volume of the lye added in step S1 is equal to the volume of the lye added in step X1.
Further, in a preferred embodiment of the present invention, the alkaline solution is sodium hydroxide to avoid introducing impurities.
Further, in the preferred embodiment of the present invention, the concentration of the alkali solution is 100-200 g/L. The sodium hydroxide with the concentration of 100-200g/L can ensure that the hemicellulose is completely dissolved and is converted into reducing sugar solid.
Further, in a preferred embodiment of the present invention, the refractometer comprises a fully automatic refractometer or an Abbe refractometer.
Further, in a preferred embodiment of the present invention, when a refractometer is used, the room temperature is set to 20 to 25 ℃, the resolution of the refractometer is 0.01%, and the measurement accuracy is ± 0.05%.
The method for measuring the content of the hemicellulose in the xylo-oligosaccharide produced by the viscose wastewater has the beneficial effects that:
(1) the invention solves the problem that in the detection method for determining the content of hemicellulose in the xylo-oligosaccharide raw material by adopting a redox method, the accuracy of a detection result is influenced by factors such as complex detection process, long oxidation reaction time, incomplete oxidation reaction, temperature fluctuation and the like. In the invention, the content of reducing sugar solid in the xylo-oligosaccharide raw material treated by alkali liquor is detected by adopting a refraction method, and the content of hemicellulose in the raw material is calculated by using a linear regression equation, so that the problem of unstable experimental data is solved, and the accuracy of the detected data is improved;
(2) the method has the advantages that the detection of the content of the hemicellulose in the raw materials in the production process of the xylo-oligosaccharide is rapid, the detection period is short, the detection period is shortened by about 80min compared with the traditional detection method, and the control of the production process can be guided in time; meanwhile, the method is simple to operate and high in practicability, does not need to newly add detection equipment and a detection field, and is low in detection cost;
(3) the invention has wide application range and strong practicability; the detection method can be used for detecting the content of the hemicellulose in the raw materials for producing the xylo-oligosaccharide, detecting the content of the hemicellulose in the production process of the xylo-oligosaccharide, and detecting the content of the hemicellulose in other processes, namely suitable for all processes for detecting the content of the hemicellulose.
Drawings
FIG. 1 is a graph of a standard curve in example 2;
FIG. 2 is a standard graph of example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The embodiment provides a method for measuring the content of hemicellulose in xylooligosaccharide produced by viscose wastewater, which comprises the following steps:
1) establishing a standard curve: s1 preparation: weighing 100g of hemicellulose, adding into 1L of distilled water, and stirring until the hemicellulose is completely dissolved to obtain a standard substance with the concentration of 100 g/L; then, the standard substance is diluted into 5 standard solutions with different concentrations, namely 50g/L, 60g/L, 70g/L, 80g/L and 90 g/L; then respectively taking 50mL of standard solution, respectively adding 10mL of alkali liquor with the concentration of 200g/L, and standing for 8 min; s2 measurement: respectively detecting the content of solid reducing sugar generated in the standard solution by using a refractometer, and recording data shown in table 1;
TABLE 1
| Concentration of Standard solution (g/L) | 50 | 60 | 70 | 80 | 90 |
| Content of reducing sugar solid (%) | 12.09 | 12.85 | 13.76 | 14.52 | 15.41 |
S3, linear regression equation: establishing a standard curve by using a unary linear regression method according to the data recorded in step S2 as shown in fig. 1, and obtaining a linear regression equation Y of 0.0831X +7.909 (R)20.999), wherein Y represents the reducing sugar solid content and X represents the hemicellulose content;
2) sampling sample liquid: collecting viscose waste water in viscose fiber production, then recovering sodium hydroxide in the viscose waste water by adopting a conventional nanofiltration technology in the field, using the remaining trapped fluid to produce xylo-oligosaccharide, and taking 50mL of trapped fluid as sample fluid;
3) and (3) sample liquid detection: x1 pretreatment: adding 10mL of sodium hydroxide solution with the concentration of 200g/L into the sample solution, and standing for 8 min; x2 measurement: detecting the content of solid reducing sugar generated in the sample liquid by using an Abbe refractometer, and recording data; x3: repeating the step X2 4 times to record data;
4) calculating the content of hemicellulose in the sample liquid: y1: according to the data of X2 and X3, the average value of the solid content of reducing sugar, namely the value of Y: y2: according to the linear regression equation Y of step S3 ═ 0.0831X +7.909(R20.999), the value Y is entered and the content of hemicellulose in the sample liquid, i.e. the value X, is calculated.
20 groups of sample liquids were taken and measured by the steps 2) to 4) (refraction method) provided in this example and by the conventional detection method (oxidation method), and the detection results are shown in the following table 2:
TABLE 2
The results were compared according to table 2: the detection data error between the embodiment and the traditional detection method is small, the maximum error is 1.99g/L and is within the range of standard error of 3g/L, but the detection period in the embodiment is reduced by 80 +/-6 min compared with the period of the traditional detection method.
Example 2
The embodiment provides a method for measuring the content of hemicellulose in xylooligosaccharide produced by viscose wastewater, which comprises the following steps:
1) establishing a standard curve: s1 preparation: weighing 100g of hemicellulose, adding into 1L of distilled water, and stirring until the hemicellulose is completely dissolved to obtain a standard substance with the concentration of 100 g/L; then, the standard substance is diluted into 5 standard solutions with different concentrations, namely 40g/L, 50g/L, 60g/L, 70g/L and 80 g/L; then respectively taking 50mL of standard solution, respectively adding 10mL of alkali liquor with the concentration of 200g/L, and standing for 10 min; s2 measurement: respectively detecting the content of solid reducing sugar generated in the standard solution by using a refractometer, and recording data shown in table 3;
TABLE 3
| Concentration of Standard solution (g/L) | 40 | 50 | 60 | 70 | 80 |
| Content of reducing sugar solid (%) | 11.20 | 12.04 | 12.95 | 13.84 | 14.72 |
S3, linear regression equation: establishing a standard curve by using a unary linear regression method according to the data recorded in step S2 as shown in fig. 2, and obtaining a linear regression equation Y of 0.0884X +7.646 (R)20.999), wherein Y represents the reducing sugar solid content and X represents the hemicellulose content;
2) sampling sample liquid: collecting viscose waste water in viscose fiber production, then recovering sodium hydroxide in the viscose waste water by adopting a conventional nanofiltration technology in the field, using the remaining trapped fluid to produce xylo-oligosaccharide, and taking 50mL of trapped fluid as sample fluid;
3) and (3) sample liquid detection: x1 pretreatment: adding 10mL of sodium hydroxide solution with the concentration of 200g/L into the sample solution, and standing for 10 min; x2 measurement: detecting the content of solid reducing sugar generated in the sample liquid by using an Abbe refractometer, and recording data; x3: repeating the step X2 3 times to record data;
4) calculating the content of hemicellulose in the sample liquid: y1: according to the data of X2 and X3, the average value of the solid content of reducing sugar, namely the value of Y: y2: according to the linear regression equation Y in step S3 ═ 0.0884X +7.646 (R)20.999), the value Y is entered and the content of hemicellulose in the sample liquid, i.e. the value X, is calculated.
20 groups of sample liquids were measured by the steps 2) to 4) (refraction method) provided in this example and by the conventional detection method (oxidation method), and the results are shown in the following table 4:
TABLE 4
Alignment according to table 4 results: the detection data error between the embodiment and the traditional detection method is small, the maximum error is 1.91/L and is within the range of standard error of 3g/L, but the detection period in the embodiment is reduced by 80 +/-3 min compared with the period of the traditional detection method.
Example 3
On the basis of example 1, the standard solution and the sample solution were treated with alkali solutions of different concentrations, and the statistics of the results are shown in the following table 5:
TABLE 5
On the basis of table 5, further analysis yields: when the concentration of the sodium hydroxide solution is less than 100-200g/L, the hemicellulose in the standard solution and the sample solution is not completely dissolved into soluble reducing sugar, and the undissolved hemicellulose is in a suspension state; when a refractometer is used for detecting the solid content of reducing sugar, only the dissolved hemicellulose content can be detected, and the detected solid content of reducing sugar is lower than the actual solid content of reducing sugar, so that the hemicellulose measurement result is lower, and the detection accuracy is seriously influenced.
When the concentration of the sodium hydroxide solution is 100-200g/L, the hemicellulose in the standard solution and the sample solution is completely dissolved into soluble reduced sugar; and detecting the solid content of the reducing sugar by using a refractometer, and establishing a standard curve, wherein the solid content of the reducing sugar and the content of hemicellulose are in a linear relation at the moment, so that the detection accuracy is ensured.
When the concentration of the sodium hydroxide solution is more than 100-200g/L, although the hemicellulose in the standard solution and the sample solution is completely dissolved into soluble reducing sugar, the redundant sodium hydroxide solid can be detected by a refractometer, and the sodium hydroxide solid interferes with the reducing sugar solid, so that the solid content value is higher than the actual value, and the hemicellulose content result is higher, thereby seriously affecting the detection accuracy.
In conclusion, the method for measuring the content of the hemicellulose in the xylo-oligosaccharide produced by the viscose wastewater provided by the invention is adopted; the method comprises the steps of taking viscose waste water after alkali removal as a raw material, wherein the raw material contains a large amount of hemicellulose and a small amount of sodium hydroxide, detecting the content of solid reducing sugar by a refraction method according to the principle that the hemicellulose is dissolved into solid reducing sugar under an alkaline condition, establishing a standard curve, calculating the relation between the content of the solid reducing sugar and the content of the hemicellulose by using a linear regression equation, finally calculating the content of the hemicellulose in a xylo-oligosaccharide raw material by using the linear regression equation, accurately calculating the addition of xylanase, and controlling the production process of the xylo-oligosaccharide; the invention has the advantages of high detection accuracy, short period, convenient operation and low cost.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for measuring the content of hemicellulose in xylo-oligosaccharide produced by viscose wastewater is characterized by comprising the following steps: the method comprises the following steps:
1) establishing a standard curve:
s1 preparation: weighing hemicellulose, adding the hemicellulose into distilled water, and stirring until the hemicellulose is completely dissolved to obtain a standard substance with the concentration of 100-; then diluting the standard substance into at least 5 standard solutions with different concentrations, then respectively taking the same amount of standard solution, respectively adding the same amount of alkali liquor according to the volume ratio of 1:5 to the standard solution, and standing for 5-10 min;
s2 measurement: respectively detecting the content of solid reducing sugar generated in the standard solution by using a refractometer, and recording data;
s3, linear regression equation: establishing a standard curve by adopting a unary linear regression method according to the data recorded in the step S2 to obtain a linear regression equation Y = aX + b, wherein Y represents the solid content of reducing sugar, and X represents the content of hemicellulose;
2) sampling sample liquid: taking a sample liquid containing hemicellulose with unknown content; the sample solution is trapped fluid obtained by recovering sodium hydroxide from viscose waste water, wherein the concentration of hemicellulose in the trapped fluid is 90-110g/L, and the concentration of sodium hydroxide is 40-45 g/L;
3) and (3) sample liquid detection:
x1 pretreatment: adding the alkali liquor into the sample liquid according to the volume ratio of the alkali liquor to the sample liquid being 1:5, and standing for 5-10 min; the concentration of the alkali liquor is 100-200 g/L;
x2 measurement: detecting the content of solid reducing sugar generated in the sample liquid by using a refractometer, and recording data;
x3: repeating the step X2 for 2-5 times, and recording data;
4) calculating the content of hemicellulose in the sample liquid:
y1: obtaining the average value of the solid content of reducing sugar, namely the Y value according to the data of X2 and X3;
y2: and substituting the Y value according to the linear regression equation in the step S3 and calculating the content of the hemicellulose in the sample liquid, namely the X value.
2. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1, wherein the method comprises the following steps: in step S1, the hemicellulose is experimentally pure.
3. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1, wherein the method comprises the following steps: the standard solution and the sample solution have the same volume.
4. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1, wherein the method comprises the following steps: the volume of the alkali solution added in step S1 is equal to the volume of the alkali solution added in step X1.
5. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1 or 4, wherein the method comprises the following steps: the alkali liquor is sodium hydroxide.
6. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1, wherein the method comprises the following steps: the refractometer comprises a full-automatic refractometer or an Abbe refractometer.
7. The method for measuring the content of hemicellulose in the xylo-oligosaccharide produced by viscose wastewater according to claim 1, wherein the method comprises the following steps: when the refractometer is used, the room temperature is set to be 20-25 ℃, the resolution of the refractometer is 0.01%, and the measurement precision is +/-0.05%.
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