LU102166B1 - Measuring method for content of catalyst in furfural residue - Google Patents
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- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention discloses a measuring method for a content of a catalyst in a furfural residue, including the following steps: SI: burning a furfural residue sample; S2: adding water to filter a burning residue of the furfural residue sample in SI; S3: performing a precipitation reaction on a filtrate obtained in S2; S4: filtering a suspension obtained in S3; S5: washing a filter cake obtained in S4; S6: drying a filter cake obtained in S5; and S7: calculating the content of KHS04 in the furfural residue sample according to a precipitate weight in S6. In a measuring process of the measuring method according to the present invention, no expensive high-end instrument is needed, and only conventional, inexpensive instruments and materials, such as a balance, a muffle furnace, a funnel, and filter paper, are needed. In the method of the present invention, a furfural residue sample needs to be burned only once, and second burning is not needed, so that systematic errors caused by the second burning are eliminated. The present invention has high measuring accuracy, and a recovery rate of a catalyst in the sample may reach 99%.
Description
P100581LU00 LUtozies | FURFURAL RESIDUE | BACKGROUND | Technical Field | The present invention relates to a measuring method, and specifically, to a measuring | method for a content of a catalyst in a furfural residue. . Related Art | Furfural is an important fine chemical product with a wide range of uses. At present, the .
furfural is mainly produced by catalyzing hydrolysis of biomass, such as corncobs, using | sulfuric acid as a catalyst. However, disadvantages of the sulfuric acid catalyst are high | toxicity and strong corrosivity. Sulfuric acid exists in a solid residue (commonly known as a È furfural residue) after the furfural is extracted and is not recycled. In industry, the furfural |! residue is generally used as boiler fuel. In a combustion process, sulfuric acid is decomposed | into sulfur trioxide and is exhausted out of a furnace chamber along with flue gas. If the flue | gas is not desulfurized and purified, sulfur trioxide may cause air pollution. To overcome the | disadvantages of high toxicity and strong corrosivity of sulfuric acid, the furfural is prepared | by catalyzing hydrolysis of biomass, such as corncobs, with potassium bisulfate, and | potassium bisulfate remaining in the furfural residue after the hydrolysis is recovered and .
recycled. Therefore, a measuring method for a content of potassium bisulfate in a furfural | residue is needed to timely obtain an initial content of potassium bisulfate in the furfural | residue and a trace content of potassium bisulfate remaining in the furfural residue after Ë potassium bisulfate is recovered in a process of preparing the furfural, and also obtain a |) recovery rate of a catalyst. .
The patent CN201911098710.1 discloses a measuring method for a content of sodium | hydrogen sulfate as a catalyst in a furfural residue. Although this method can also be used for | measuring a content of a potassium bisulfate catalyst in a furfural residue, the method Ë requires operations of two-time high-temperature burning, in which there are disadvantages | of high energy consumption and time-consuming analysis. In addition, in a stage in which | water in a sample is evaporated to almost dryness during the second high-temperature ı burning, salt particles in the sample may be spattered, which is prone to cause a trace loss of | the sample, resulting in systematic errors in the measurement. To overcome the foregoing | disadvantages, the present invention adopts an analysis method combining one-time burning | and a precipitation reaction, which not only can overcome the disadvantages of the foregoing '
analysis method, but also has higher measuring accuracy. LU102166 | SUMMARY .
An objective of the present invention is to provide a measuring method for a content of a | catalyst in a furfural residue. In a measuring process, no expensive high-end instrument is | needed, and only conventional, inexpensive instruments and materials, such as a balance, a | muffle furnace, a funnel, and filter paper, are needed. In the method of the present invention, | a furfural residue sample needs to be burned only once, and second burning is not needed, so | that systematic errors caused by the second burning are eliminated. The present invention | has high measuring accuracy, and a recovery rate of a catalyst in the sample may reach 99%, | The measuring method of the present invention is easy to operate, has low operating costs | and a short analysis period, and is particularly suitable for use in small and medium | enterprises and laboratories lacking high-end instruments. | The objective of the present invention can be achieved through the following technical | solutions: | A measuring method for a content of a catalyst in a furfural residue is provided, | including the following steps: . S1: burning a furfural residue sample; | S2: adding water to filter a burning residue of the furfural residue sample in S1; S3: performing a precipitation reaction on a filtrate obtained in S2; | S4: filtering a suspension obtained in S3; | S5: washing a filter cake obtained in 54; . S6: drying a filter cake obtained in SS; and . S7: calculating the content of KHSO4 in the furfural residue sample according to a | precipitate weight in S6. : Further, SI specifically includes: sufficiently drying the furfural residue containing | catalyst potassium bisulfate at a temperature of 105°C to remove moisture to obtain a dried | furfural residue; weighing the dried furfural residue sample by using a clean corundum | combustion boat, a mass range of the sample being 0.4 g<™ <0.6 g; placing the combustion | boat holding the sample in a muffle furnace heated to a preset temperature, the preset | temperature ranging from 600°C to 700°C; igniting and burning the sample, after naked | flames go out, closing a furnace door, and after the temperature of the muffle furnace returns | to the preset temperature, further maintaining the burning for 1-1.5 h to completely burn out | organic substances in the sample; converting potassium bisulfate in the sample into | potassium sulfate through reactions (1) and (2), and mixing potassium sulfate with insoluble LU102166 | ash formed of the furfural residue through combustion; and taking the combustion boat out | of the muffle furnace and cooling the combustion boat to room temperature, where | condensation polymerization: 2KHSO, — K2820, + H,0 (1); | decomposition reaction: K,820, — K,80, + SO, 1 (2); and | total reaction is 2KHSO, > K,S0, +80, T+H,0 (3) | Further, S2 specifically includes: measuring out 10 mL deionized water, and adding the | deionized water at the same amount to the combustion boat cooled to room temperature in | S1 in three times; after the deionized water is added each time, fully stirring to fully dissolve | potassium sulfate in the combustion boat; transferring the potassium sulfate solution in the | combustion boat together with the insoluble ash into a clean beaker; and after the transfer is | completed, filtering and separating a solid-liquid mixture in the beaker to remove the | insoluble ash and obtain a filtrate in which potassium sulfate is dissolved. | Further, S3 specifically includes: dropwise adding a sufficient amount of a barium | chloride solution to the filtrate of potassium sulfate obtained in S2 to ensure that all sulfate . ions in the filtrate of potassium sulfate are precipitated as barium sulfate, to obtain a | suspension of barium sulfate, where | precipitation reaction: K,50, + BaCl, —> BaSO, + +2KCI (4); and | the concentration of the barium chloride solution ranges from 0.1 to 0.5 mol/L .
Further, S4 specifically includes: filtering the suspension obtained in S3, and adding 1-2 | drops of the barium chloride solution to the filtrate, where if the filtrate becomes turbid, the , barium chloride solution added in S3 is insufficient, and the test needs to be repeated, and | when the test is repeated, the amount of the barium chloride solution added in S3 needs to be | increased to ensure that sulfate in the potassium sulfate solution is completely precipitated; if Ë the filtrate does not become turbid, the barium chloride solution added in S3 is sufficient, | and the following operation steps are performed; and filter paper for filtering the suspension | is three-layered slow filter paper. | Further, S5 specifically includes: washing and filtering, by using the deionized water, : the filter cake of barium sulfate obtained in S4, and adding 1 drop of a 0.1 mol / L dilute | solution of silver nitrate to the filtrate, where if the filtrate becomes turbid, continuously | washing and filtering the filter cake until a new filtrate does not become turbid when the | silver nitrate solution is dropwise added to the filtrate, indicating that potassium chloride and | barium chloride in the precipitate filter cake are washed away, and the following operation LU102166 | steps are performed. | Further, S6 specifically includes: placing the precipitate filter cake obtained in SS into a | drying oven at a temperature of 105°C, and drying for 30-60 minutes, to fully remove | moisture. | Further, S7 specifically includes: weighing the dried filter cake obtained in S6 to obtain | the weight of the barium sulfate precipitate, recorded as 2; and obtaining a percentage | content of KSC; in the furfural residue sample according to stoichiometric relationships | of reactions (1)-(4), where the percentage content is: | Myyso, % "37,5 Mi +m, x100% | 230s (5) | where M maso, is a molar mass of barium sulfate, and is equal to 233.4 g/mol, and | Maso, is a molar mass of KES, , and is equal to 136.2 & /m ol, and | substituting the percentage content into formula (5) to obtain: | Maso, % =1.167x 2x 100% Ë Mr (6). : The present invention has the following beneficial effects: |
1. In a measuring process of the measuring method according to the present invention, : no expensive high-end instrument is needed, and only conventional, inexpensive instruments À and materials, such as a balance, a muffle furnace, a funnel, and filter paper, are needed. In ; the method of the present invention, a furfural residue sample needs to be burned only once, | and second burning is not needed, so that systematic errors caused by the second burning are | eliminated. The present invention has high measuring accuracy, and a recovery rate of a | catalyst in the sample may reach 99%. |
2. The measuring method of the present invention is easy to operate, has low operating | costs and a short analysis period, and is particularly suitable for use in small and medium | enterprises and laboratories lacking high-end instruments. | DETAILED DESCRIPTION | The following clearly and completely describes the technical solutions in the | embodiments of the present invention with reference to the embodiments of the present invention. Apparently, the described embodiments are merely some but not all of the embodiments of the present invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative LU102166 | efforts shall fall within the protection scope of the present invention. | A measuring method for a content of a catalyst in a furfural residue includes the | following steps. | S1: Burn a furfural residue sample. | The furfural residue containing catalyst potassium bisulfate is sufficiently dried at a | temperature of 105°C to remove moisture to obtain a dried furfural residue.
The dried | furfural residue sample (g) is weighed by using a clean corundum combustion boat, a | mass range of the sample being 0.4 g<"" <0.6 g.
The combustion boat holding the sample is | placed in a muffle furnace heated to a preset temperature, the preset temperature ranging | from 600°C to 700°C.
The sample is ignited and burned, after naked flames go out, a fumace | door is closed, and after the temperature of the muffle furnace returns to the preset | temperature, the burning is maintained for 1-1.5 h to completely burn out organic substances : in the sample.
Potassium bisulfate in the sample is converted into potassium sulfate through | reactions (1) and (2), and potassium sulfate is mixed with insoluble ash formed of the . furfural residue through combustion.
The combustion boat is taken out of the muffle furnace À and cooled to room temperature. . Condensation polymerization: 2KHSO, > K2520, + H,0 (1) : Decomposition reaction: K28207 = K,50, + SO, 1 (2) | Total reaction: 7KFSO, > K,50, + SO; T+H,0 (3) | S2: Add water to filter a burning residue of the furfural residue sample. | 10 mL deionized water is accurately measured out by using a measuring cylinder and | added to the combustion boat cooled to room temperature in Sl in three times | (approximately 3 mL each time). After the deionized water is added each time, the mixture is : stirred fully to fully dissolve potassium sulfate in the combustion boat.
The potassium sulfate | solution in the combustion boat together with the insoluble ash is transferred into a clean | beaker.
After the transfer is completed, a solid-liquid mixture in the beaker is filtered and | separated, to remove the insoluble ash.
A filtrate in which potassium sulfate is dissolved is | obtained. / $3: Perform a precipitation reaction on a filtrate obtained in S2. A sufficient amount of a barium chloride solution is added dropwise to the filtrate of potassium sulfate obtained in S2 to ensure that all sulfate ions in the filtrate of potassium sulfate are precipitated as barium sulfate, to obtain suspension of barium sulfate is obtained.
LU102166 | À concentration of the barium chloride solution ranges from 0.1 to 0.5 mol/L | Precipitation reaction: £2504 + BaCl, — BaSO, L+2KCI (4) | S4: Filter a suspension obtained in S3. | The suspension obtained in S3 is filtered to obtain a filter cake and a filtrate.
Because | the resultant precipitate is very fine, three-layered slow filter paper is used for filtering. 1-2 A drops of the barium chloride solution is added to the filtrate.
If the filtrate becomes turbid, | the barium chloride solution added in S3 is insufficient, and the test needs to be repeated. | When the test is repeated, the amount of the barium chloride solution added in S3 needs to | be increased to ensure that sulfate in the potassium sulfate solution is completely precipitated. | If the filtrate does not become turbid, the barium chloride solution added in S3 is sufficient, | and the operation of S5 is performed. | S5: Wash a filter cake obtained in S4. | The filter cake of barium sulfate obtained in S4 is washed and filtered by using a . sufficient amount of the deionized water. 1 drop of a 0.1 mol/L dilute solution of silver | nitrate is added to the filtrate.
If the filtrate becomes turbid, the filter cake is continuously Î washed and filtered until a new filtrate does not become turbid when the silver nitrate | solution is added dropwise to the filtrate, indicating that potassium chloride and barium | chloride in the precipitate filter cake are washed away, and the operation of S6 may be | performed. | S6: Dry a filter cake obtained in S5. | The precipitate filter cake obtained in S5 is placed into a drying oven at a temperature of | 105°C and dried for 30-60 minutes, to fully remove moisture. | S7: Calculate a content of ÉHSO; in the furfural residue sample according to a | precipitate weight. | The dried filter cake obtained in S6 is weighed to obtain the weight of the barium sulfate | precipitate, recorded as "2 (g). A percentage content of KHSO, in the furfural residue sample is obtained according to stoichiometric relationships of reactions (1)-(4), where the percentage content is: Ms, % "7 2x M py, + My 100% (us (5) where M250, is a molar mass of barium sulfate, and is equal to 233.4 g/mol, and
Mino, is a molar mass of KÆSO,_ and is equal to 136.2 8/mol LU102166 | The percentage content is substituted into formula (5) to obtain: | Mynso, % = 1.167x 2x 100% | Example 1 | The furfural residue containing catalyst potassium bisulfate of a known concentration | was dried at a temperature of 105°C for 1 h to fully remove free moisture to obtain the dried | furfural residue, where an actual content of potassium bisulfate was 12.050%. The dried | furfural residue sample was weighed by using a 40 mmx60 mmx100 mm dry corundum | combustion boat, and the mass was "1 =0.5006 g. The combustion boat holding the sample | was placed in the muffle furnace pre-heated to 650°C, and the sample was ignited and | burned. After naked flames went out, the furnace door was closed. After the temperature of | the muffle furnace returned to 650°C, the burning was maintained at 650°C for 1 h. Then, | the combustion boat was taken out of the muffle furnace and cooled to room temperature in a | dry environment. | 10 mL deionized water was accurately measured out and added to the combustion boat | in three times (approximately 3 mL each time). After the deionized water was added each | time, the mixture was stirred fully to fully dissolve potassium sulfate in the combustion boat. .
The potassium sulfate solution in the combustion boat together with the insoluble ash was | transferred into a clean beaker. After the transfer was completed, a solid-liquid mixture in the : beaker was filtered and separated. The filtrate was completely transferred into the beaker, | and a sufficient amount of a 0.1 M0//L barium chloride solution was added to precipitate | all sulfate ions in the filtrate. The precipitate suspension was filtered, and the filter cake was ; fully washed with the deionized water, until the filtrate did not become turbid when tested | with a 0.1 mol/L silver nitrate solution. The filter cake was placed into the drying oven at ; a temperature of 105°C for drying for 1 h to obtain the dried precipitate filter cake. The | precipitate weight obtained by weighing was "2 =0.0518 g. The content of potassium | bisulfate in the sample calculated by substituting "2 and ™ into formula (6) was |
12.052%, and a relative deviation from the actual content was 0.17%. / Example 2 | The furfural residue containing catalyst potassium bisulfate of a known concentration | was dried at a temperature of 105°C for 1 h to fully remove free moisture to obtain the dried | furfural residue, where an actual content of potassium bisulfate was 28.705%. The dried LU102166 | furfural residue sample was weighed by using a 40 mmx60 mmx100 mm dry corundum | combustion boat, and the mass was "1=0.5618 g.
The following operations were the same | as those in Example 1. Finally, the precipitate weight obtained by weighing was ‘=0.1382 | g.
The content of potassium bisulfate in the sample calculated by substituting "2 and A | into formula (6) was 28.707%, and a relative deviation from the actual content was 0.70%. | Example 3 |
The furfural residue containing catalyst potassium bisulfate of a known concentration ;
was dried at a temperature of 105°C for 1 h to fully remove free moisture to obtain the dried | furfural residue, where an actual content of potassium bisulfate was 6.385%. The dried | furfural residue sample was weighed by using a 40 mmx60 mmx100 mm dry corundum | combustion boat, and the mass was ™=0.5209 g.
The following operations were the same | as those in Example 1. Finally, the precipitate weight obtained by weighing was 72=0.0285 | g.
The content of potassium bisulfate in the sample calculated by substituting ”% and 74 | into formula (6) was 6.389%, and a relative deviation from the actual content was 0.63%, | In the descriptions of this specification, a description of a reference term such as "an | embodiment", "an example", or "a specific example" means that a specific feature, structure, ; material, or characteristic that is described with reference to the embodiment or the example | is included in at least one embodiment or example of the present invention.
In this | specification, exemplary descriptions of the foregoing terms do not necessarily refer to a | same embodiment or example.
In addition, the described specific features, structures, | materials, or features can be combined in a proper manner in any one or more embodiments | or examples. | The basic principles, main features and advantages of the present invention are shown | and described above.
Persons skilled in the art should understand that the present invention | is not limited by the foregoing embodiments, descriptions in the foregoing embodiments and | the specification merely describe the principles of the present invention, various changes and | improvements may be made to the present invention without departing from the spirit and | scope of the present invention, and such changes and improvements shall all fall within the | protection scope of the present invention.
Claims (8)
1. A measuring method for a content of a catalyst in a furfural residue, comprising the | following steps: | S1: burning a furfural residue sample; | S2: adding water to filter a burning residue of the furfural residue sample in S1; | S3: performing a precipitation reaction on a filtrate obtained in S2; | S4: filtering a suspension obtained in S3; | S5: washing a filter cake obtained in S4; à S6: drying a filter cake obtained in S5; and | S7: calculating the content of KHSO4 in the furfural residue sample according to a | precipitate weight in S6. |
2. The measuring method for a content of a catalyst in a furfural residue according to ° claim 1, wherein S1 specifically comprises: sufficiently drying the furfural residue | containing catalyst potassium bisulfate at a temperature of 105°C to remove moisture to | obtain a dried furfural residue; weighing the dried furfural residue sample ” by using a | clean corundum combustion boat, a mass range of the sample being 0.4 g<”" <0.6 g; placing : the combustion boat holding the sample in a muffle furnace heated to a preset temperature, .
the preset temperature ranging from 600°C to 700°C; igniting and burning the sample, after ‘ naked flames go out, closing a furnace door, and after the temperature of the muffle furnace | returns to the preset temperature, further maintaining the burning for 1-1.5 h to completely | burn out organic substances in the sample; converting potassium bisulfate in the sample into i potassium sulfate through reactions (1) and (2), and mixing potassium sulfate with insoluble ; ash formed of the furfural residue through combustion; and taking the combustion boat out É of the muffle furnace and cooling the combustion boat to room temperature, wherein | condensation polymerization: 2KHSO, —> K28,0; + H,0 (5 / decomposition reaction: K25,0, — K,80,+50, 1 (2); and | total reaction: 2KHSO, => K,S0,+80, T+H,0 3). |
3. The measuring method for a content of a catalyst in a furfural residue according to | claim 2, wherein S2 specifically comprises: measuring out 10 mL deionized water, and | adding the deionized water at the same amount to the combustion boat cooled to room | temperature in S1 in three times; after the deionized water is added each time, fully stirring | to fully dissolve potassium sulfate in the combustion boat; transferring the potassium sulfate | U102166 | solution in the combustion boat together with the insoluble ash into a clean beaker; and after | the transfer is completed, filtering and separating a solid-liquid mixture in the beaker to | remove the insoluble ash and obtain a filtrate in which potassium sulfate is dissolved. .
4. The measuring method for a content of a catalyst in a furfural residue according to | claim 3, wherein S3 specifically comprises: dropwise adding a sufficient amount of a barium | chloride solution to the filtrate of potassium sulfate obtained in S2 to ensure that all sulfate | ions in the filtrate of potassium sulfate are precipitated as barium sulfate, to obtain a ° suspension of barium sulfate, wherein | precipitation reaction: K,50, + BaCl, — BaSO, 4 +2KCI (4) . the concentration of the barium chloride solution ranges from 0.1 to 0.5 mol/L |
5. The measuring method for a content of a catalyst in a furfural residue according to ; claim 4, wherein S4 specifically comprises: filtering the suspension obtained in S3, and . adding 1-2 drops of the barium chloride solution to the filtrate, wherein if the filtrate . becomes turbid, the barium chloride solution added in S3 is insufficient, and the test needs to . be repeated, and when the test is repeated, the amount of the barium chloride solution added in 83 needs to be increased to ensure that sulfate in the potassium sulfate solution is : completely precipitated; if the filtrate does not become turbid, the barium chloride solution | added in S3 is sufficient, and the following operation steps are performed; and filter paper Ë for filtering the suspension is three-layered slow filter paper. |
6. The measuring method for a content of a catalyst in a furfural residue according to | claim 5, wherein S5 specifically comprises: washing and filtering, by using the deionized | water, the filter cake of barium sulfate obtained in S4, and adding 1 drop of a 0.1 mol/L | dilute solution of silver nitrate to the filtrate, wherein if the filtrate becomes turbid, the filter | cake is continuously washed and filtered until a new filtrate does not become turbid when | the silver nitrate solution is dropwise added to the filtrate, indicating that potassium chloride | and barium chloride in the precipitate filter cake are washed away, and the following | operation steps are performed. /
7. The measuring method for a content of a catalyst in a furfural residue according to claim 6, wherein S6 specifically comprises: placing the precipitate filter cake obtained in S5 into a drying oven at a temperature of 105°C, and drying for 30-60 minutes, to fully remove moisture.
8. The measuring method for a content of a catalyst in a furfural residue according to i NN claim 7, wherein S7 specifically comprises: weighing the dried filter cake obtained in S6 toLU102166 . obtain the weight of the barium sulfate precipitate, recorded as 2; and obtaining a | percentage content of KHSO, in the furfural residue sample according to stoichiometric | relationships of reactions (1)-(4), wherein the percentage content is: | % = — 2x 2x Mgr, + My *100% |
Muso, 7° = 7 KHSO, ~ "1 0 |
BaSO, ( 5) | My. : ; ; = wherein 50%: is a molar mass of barium sulfate, and is equal to 233.4 g/mol, and |
Mguso, : KH, . | K#s0s js a molar mass of X04 and is equal to 136.2 E/ MOI; and | substituting the percentage content into formula (5) to obtain: |
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