CN216856337U - System for preparing furfural by using hemicellulose or xylose raw material liquid - Google Patents
System for preparing furfural by using hemicellulose or xylose raw material liquid Download PDFInfo
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- CN216856337U CN216856337U CN202220033110.8U CN202220033110U CN216856337U CN 216856337 U CN216856337 U CN 216856337U CN 202220033110 U CN202220033110 U CN 202220033110U CN 216856337 U CN216856337 U CN 216856337U
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 342
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 172
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 86
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000007788 liquid Substances 0.000 title claims abstract description 83
- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 81
- 239000002994 raw material Substances 0.000 title claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 95
- 238000006243 chemical reaction Methods 0.000 claims abstract description 84
- 239000003054 catalyst Substances 0.000 claims abstract description 83
- 238000000605 extraction Methods 0.000 claims abstract description 63
- 230000003068 static effect Effects 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
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- 239000012141 concentrate Substances 0.000 claims description 11
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 9
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 9
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 6
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Abstract
The utility model relates to a system for preparing furfural by utilizing hemicellulose or xylose raw material liquid, which comprises a static mixer, a reaction extraction tower and a rectifying tower system, wherein the static mixer is used for mixing the hemicellulose or xylose raw material liquid with a catalyst to obtain mixed material liquid, the reaction extraction tower is used for extracting a furfural component generated in the mixed material liquid by using an oil phase extracting agent entering from the outside to obtain an oil phase extracting agent containing the furfural component, and the rectifying tower system is used for separating the furfural component in the oil phase extracting agent containing the furfural component from the oil phase extracting agent. The utility model has high extraction efficiency, low cost and good economic benefit. In the process of preparing the furfural product by using the system, the water phase, the oil phase and the acidic ion buffer solution catalyst used in the whole production process can be recycled for multiple times, so that the energy consumption and the discharge amount of three wastes are reduced, and the yield of the furfural is improved.
Description
Technical Field
The utility model belongs to the technical field of acid catalysis and furfural preparation, and particularly relates to a system for preparing furfural by using hemicellulose or xylose raw material liquid.
Background
Biomass is not only a renewable resource, but also the most widely distributed, numerous and varied resource on earth, and has attracted considerable attention from many researchers. The research of producing high value-added compounds by taking basic platform compounds of biomass as raw materials is more and more, so the applicable production technology and production route can be applied, and the final production of high value-added products has a profound influence on the development of the biomass conversion industry.
The furfural is used as a basic platform substance of biomass, is a five-carbon compound, can be prepared by converting biomass with abundant reserves in agriculture, forestry and the like, and has wide application. Furfural is used as an important derivative compound of a furan ring system, can be used as a basic raw material to synthesize a plurality of compounds with high added values, and is expected to reduce the current dependence of China on fossil resources.
At present, most of catalysts used for preparing furfural by dehydrating hemicellulose or xylose are inorganic acids, and too much inorganic acids are used to corrode chemical equipment and are not beneficial to long-term production; on the other hand, the solid acid catalyst is also used for the reaction of preparing furfural by dehydrating hemicellulose or xylose, but the reaction system in the solid acid catalysis process is heterogeneous, so that the activation energy required by the reaction is higher, and more resources are wasted. At present, the research of China in the aspect is still in a lagging stage, and the way of developing biomass hydrolysis to prepare furfural is still far from the right.
SUMMERY OF THE UTILITY MODEL
The technical problem to be solved by the utility model is to provide a system for preparing furfural by utilizing hemicellulose or xylose raw material liquid, develop and use a liquid acidic ion buffer solution catalyst to prepare a furfural product, wherein a water phase, an oil phase and the catalyst in the preparation process can be recycled, so that the energy consumption and the discharge amount of three wastes are reduced, and the yield of furfural is improved.
The utility model is realized in this way, also provides a system for preparing furfural by using hemicellulose or xylose raw material liquid, which comprises a static mixer, a reaction extraction tower and a rectification tower system, wherein the static mixer is respectively provided with a hemicellulose or xylose raw material liquid feeding port, a catalyst feeding port and a mixed liquid discharging port, the mixed liquid discharging port is communicated with a feeding port at the upper part of the reaction extraction tower through a water phase pipeline, the upper part of the reaction extraction tower is also provided with an oil phase outlet which is convenient for an oil phase extracting agent containing furfural components in the reaction extraction tower to leave, the bottom of the reaction extraction tower is provided with an oil phase inlet which is convenient for the oil phase extracting agent to enter the reaction extraction tower, and an oil phase input pipeline is communicated with the oil phase inlet; the oil phase outlet is communicated with the feed end of the rectifying tower system through a pipeline, and a furfural collecting pipeline is arranged on the rectifying tower system and used for collecting furfural products.
Further, the rectifying tower system comprises a first rectifying tower and a second rectifying tower, the first rectifying tower is communicated with the oil phase outlet through a first pipeline, the second rectifying tower is communicated with the oil phase outlet through a second pipeline, and a furfural collecting pipeline is arranged at the bottom of the second rectifying tower system or at the top of the first rectifying tower system respectively and used for collecting furfural products.
Furthermore, a first collection port for recovering the oil phase extractant is arranged at the bottom of the first rectifying tower system, a second collection port for recovering the oil phase extractant is arranged at the bottom of the second rectifying tower system, the first collection port is communicated with the oil phase input port through a first oil phase recovery pipeline, the second collection port is also communicated with the oil phase input port through a second oil phase recovery pipeline, and a second filter and a second adsorber for removing impurities in the recovered oil phase extractant are arranged on the first oil phase recovery pipeline.
Furthermore, the first pipeline and the second pipeline are respectively communicated with the oil phase outlet through a return pipeline, and an oil phase pump is arranged on the return pipeline.
The system further comprises an evaporation system, a water phase outlet is further arranged at the bottom of the reactive extraction tower and is communicated with the feed end of the evaporation system through a discharge pipeline, a water vapor discharge port and a concentrated solution discharge port are further arranged on the evaporation system, the concentrated solution discharge port is communicated with a feed port of the static mixer through a concentrated solution pipeline, and a first filter and a first adsorber for removing impurities in the concentrated solution are respectively arranged on the concentrated solution pipeline.
Further, a discharge pump is arranged on the discharge pipeline.
Further, a first concentration pump is arranged on the concentrate pipeline between the concentrate discharge port and the first filter, and a second concentration pump is arranged on the concentrate pipeline between the first adsorber and the feed inlet of the static mixer.
Compared with the prior art, the system for preparing furfural by utilizing hemicellulose or xylose raw material liquid comprises a static mixer, a reaction extraction tower and a rectifying tower system, wherein the water phase of the reaction extraction tower is the hemicellulose or xylose raw material liquid and the catalyst which are mixed by the static mixer, the oil phase is a solution capable of extracting furfural components from the water phase, and the rectifying tower system separates the furfural components from the oil phase from which the furfural components are extracted. The utility model has high extraction efficiency, low cost and good economic benefit. In the process of preparing furfural products by using the system of the utility model, the water phase, the oil phase and the acidic ion buffer solution catalyst used in the whole production process can be recycled for a plurality of times, thereby reducing the energy consumption and the discharge amount of three wastes and improving the yield of furfural.
Drawings
FIG. 1 is a schematic diagram of a preferred embodiment of a system for producing furfural from a hemicellulose or xylose feedstock according to the present invention;
FIG. 2 is a graph showing the effect of the composition of the oil and water phases on furfural yield according to example 5 of the present invention;
figure 3 is a graphical representation of the effect of temperature and time on furfural yield for the reactions of example 6 and example 7 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and do not limit the utility model.
Referring to fig. 1, the utility model discloses a system for preparing furfural from hemicellulose or xylose raw material liquid, which comprises a static mixer 1, a reactive extraction tower 2, a first rectifying tower system 3, a second rectifying tower system 4 and an evaporation system 5. The arrows in the figure show the flowing direction of materials (including raw material liquid, mixed material liquid, water phase, oil phase, water vapor and the like) in the system.
The static mixer 1 is used for mixing hemicellulose or xylose raw material liquid and a catalyst with each other to obtain mixed material liquid, the reaction extraction tower 2 is used for extracting a furfural component generated in the mixed material liquid by using an oil phase extracting agent entering from the outside to obtain an oil phase extracting agent containing the furfural component, and the first rectifying tower system 3 and the second rectifying tower system 4 are respectively used for separating the furfural component from the oil phase extracting agent in the oil phase extracting agent containing the furfural component.
The static mixer 1 is respectively provided with a hemicellulose or xylose raw material liquid feeding hole 11, a catalyst feeding hole 12 and a mixed liquid discharging hole 13, the hemicellulose or xylose raw material liquid enters the static mixer 1 from the raw material liquid feeding hole 11, the catalyst enters the static mixer 1 from the catalyst feeding hole 12, and the hemicellulose or xylose raw material liquid and the catalyst are mixed in the static mixer to obtain mixed material liquid. The mixed liquid discharge port 13 is communicated with a feed port 21 at the upper part of the reactive extraction tower through a water phase pipeline 115, and the mixed liquid as a water phase enters the reactive extraction tower 2 from the feed port 21 at the upper part of the reactive extraction tower 2.
An oil phase outlet 22 for facilitating the oil phase extracting agent containing furfural components in the reactive extraction tower to leave is further arranged at the upper part of the reactive extraction tower 2, an oil phase inlet 23 for facilitating the oil phase extracting agent to enter the reactive extraction tower is arranged at the bottom of the reactive extraction tower 2, an oil phase input pipeline 114 is arranged to be communicated with the oil phase inlet 23, and new oil phase extracting agent enters the reactive extraction tower 2 through the oil phase input pipeline 114. The water phase flows from top to bottom along the reactive extraction tower 2, the oil phase extractant rises from bottom to top and is in countercurrent contact with the water phase in the reactive extraction tower 2, and the oil phase extractant extracts furfural components generated by furfural reaction from the water phase.
The oil phase outlet 22 is communicated with the feed end of the first rectifying tower system 3 through a first pipeline 6, and the oil phase outlet 22 is also communicated with the feed end of the second rectifying tower system 4 through a second pipeline 7. A first valve 8 and a second valve 9 are provided on the first pipe 6 and the second pipe 7, respectively. When the boiling point of the oil phase extractant is higher than that of the furfural component, the furfural component-containing oil phase extractant is conveyed to the first rectifying column system 3 through the oil phase outlet 22 and the first valve 8. When the boiling point of the oil phase extractant is lower than that of the furfural component, the furfural component-containing oil phase extractant is conveyed into the second rectification column system 4 through the oil phase outlet 22 and the second valve 9. And a furfural collecting pipeline 10 is respectively arranged at the bottom of the second rectifying tower system 4 or the top of the first rectifying tower system 3 for collecting furfural products.
And a water phase outlet 24 is also arranged at the bottom of the reactive extraction tower 2, and the water phase outlet 24 is communicated with the feeding end of the evaporation system 5 through a discharge pipeline 101. A water vapor outlet 51 and a concentrated solution outlet 52 are also arranged on the evaporation system 5, and the concentrated solution outlet 52 is communicated with the feed inlet 14 of the static mixer 1 through a concentrated solution pipeline 102. A first filter 103 and a first adsorber 104 for removing impurities in the concentrate are provided in the concentrate line 102, respectively. The concentrated solution containing the catalyst is filtered by a first filter 103 and decolorized by a first adsorber 104 in order from a concentrated solution discharge port 52 provided at the bottom of the evaporation system 5 to remove impurities, and then is sent to the static mixer 1.
The evaporation system 5 evaporates the input water phase, the water in the water phase is discharged in a gaseous state from a water vapor discharge port 51 at the top of the evaporation system 5, and the water vapor is condensed and used for preparing the hemicellulose or xylose raw material liquid. A water vapor discharge pipe 116 is provided to communicate with the water vapor discharge port 51.
A discharge pump 105 is provided on the discharge conduit 101. A first concentration pump 106 is provided in the concentrate line 102 between the concentrate discharge port 52 and the first strainer 103, and a second concentration pump 107 is provided in the concentrate line 102 between the first adsorber 104 and the feed port 14 of the static mixer 1. The first pipeline 6 and the second pipeline 7 are respectively communicated with the oil phase outlet 22 through a return pipeline 108, and an oil phase pump 109 is arranged on the return pipeline 108.
The bottom of the first rectifying tower system 3 is provided with a first recovered oil phase extractant collecting port 31, the top of the second rectifying tower system 4 is provided with a second recovered oil phase extractant collecting port 41, the first recovered oil phase extractant collecting port 31 is communicated with the oil phase input port 23 through a first oil phase recovery pipeline 110, and the second recovered oil phase extractant collecting port 41 is also communicated with the oil phase input port 23 through a second oil phase recovery pipeline 111. A second filter 112 and a second adsorber 113 for removing impurities in the recovered oil-phase extraction agent are provided in the first oil-phase recovery line 110.
The following examples further illustrate the preparation of the acidic ion buffer catalyst of the present invention and the system and method for preparing furfural using the catalyst.
Example 1
The first embodiment of the preparation method of the acidic ion buffer solution catalyst comprises the following steps:
the molar ratio of ammonium sulfate to sulfuric acid is 1: 1.1 the preparation of acidic ionic buffer solution catalyst is carried out, the specific experimental process is as follows: 3.3g of ammonium sulfate solid is weighed, dissolved in 5mL of deionized water and subjected to ultrasonic treatment for 10min, so that the ammonium sulfate solid is uniformly dispersed in the water to obtain an ammonium sulfate solution. Then, 2.7g of 98% concentrated sulfuric acid was added dropwise to the ammonium sulfate solution and sufficiently stirred for 2 hours to obtain a colorless solution, i.e., an acidic ionic buffer catalyst, which will be referred to as catalyst a hereinafter. Changing the ratio of ammonium sulfate and 98% concentrated sulfuric acid to be 1: 1.08, 1: 1.06, 1: 1.04, 1: 1.02 and 1: 1 an acidic ionic buffer catalyst (hereinafter, abbreviated as catalyst) was synthesized, respectively, and abbreviated as catalysts B, C, D, E and F, respectively.
Example 2
The first embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) catalysts A, B, C, D, E and F prepared in example 1 were added to glass pressure tubes, respectively, in an amount of 50% of the mass of xylose substrate, and the volume ratio of oil phase to water phase was 4: 1, the xylose concentration is 0.5 kg/L.
(2) And (3) putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the furfural yield of the oil phase through a gas chromatograph, and analyzing the xylose conversion rate of the water phase through a high performance liquid chromatograph with a differential detector.
A method for analyzing xylose by using a high performance liquid chromatograph and a method for measuring furfural by using a Gas Chromatography (GC) are as follows: calculated using the ratio of the areas of the hemicellulose or xylose and furfural (FF) peaks, with naphthalene as the reference. The same is as follows.
The determination shows that when the addition amount of the catalyst is 50 percent of the mass of the xylose substrate, the yield Y of the furfuralFFAs shown in table 1 below:
TABLE 1 influence of catalysts of different feed ratios on the yield of furfural (xylose substrate)
| Serial number | A | B | C | D | E | F |
| YFF(％) | 85.0 | 76.2 | 73.6 | 70.0 | 66.8 | 60.2 |
As is clear from Table 1, when catalyst A was used, the production of furfural was confirmedYield YFFThe maximum is 85.0%.
Example 3
The second embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) respectively weighing 10%, 15%, 20%, 25%, 30%, 40%, 50%, 60%, 70% and 80% of ionic buffer solution catalyst A by mass of xylose substrate, adding the ionic buffer solution catalyst A into a glass pressure resistant tube, wherein the proportion of an oil phase to a water phase is 4: 1, the xylose concentration is 0.5 kg/L.
(2) And (3) putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
The measured yields of furfural prepared by xylose dehydration catalyzed by catalysts a with different masses are shown in table 2:
TABLE 2 influence of the amount of catalyst A on the yield of furfural (xylose substrate)
| Amount of catalyst A | 10％ | 15％ | 20％ | 25％ | 30％ | 40％ | 50％ | 60％ | 70％ | 80％ |
| YFF(％) | 60.2 | 65.4 | 68.9 | 68.9 | 79.0 | 84.6 | 85.0 | 64.8 | 69.2 | 66.8 |
As is clear from Table 2, when catalysts A having different masses were used and the amount of the catalyst was 50%, the yield Y of furfural was found to beFFThe maximum is 85.0%.
Example 4
The third embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) catalyst a prepared in example 1 was placed in a glass pressure tube, the ratio of oil phase to water phase was 4: 1, the addition amount of the catalyst is 50 percent of the mass of the xylose substrate.
(2) Respectively weighing 0.3kg/L, 0.4kg/L, 0.5kg/L, 0.6kg/L and 0.7kg/L of xylose, adding into the system in the step (1), putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
It was determined that when the xylose concentrations were 0.3kg/L, 0.4kg/L, 0.5kg/L, 0.6kg/L and 0.7kg/L, the furfural yields were 42.1%, 43.5%, 85.0%, 67.5% and 62.0%, respectively. When the xylose concentration is 0.5kg/L, the yield of the furfural is 85.0 percent at the maximum.
Example 5
The fourth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) the catalyst A prepared in example 1 was placed in a glass pressure tube, the amount of the catalyst added was 50% of the mass of the xylose substrate, and the xylose concentration was 0.5 kg/L.
(2) Respectively weighing the oil phase and the water phase in a ratio of 2: 1. 3: 1. 4: 1. 5: 1 and 6: 1, adding the glass pressure-resistant pipe into the system in the step (1), placing the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and taking an upper oil phase and a lower water phase to detect the yield of furfural and the conversion rate of xylose after the pressure-resistant pipe is cooled to room temperature.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
The results are shown in fig. 2, when the ratio of oil phase to water phase is 2: 1. 3: 1. 4: 1. 5: 1 and 6: at 1, the yields of furfural were 65.4%, 75.2%, 85.0%, 73.5%, and 60.3%, respectively. When the ratio of oil phase to water phase is 4: at 1, the yield of furfural was up to 85.0%.
Example 6
A fifth embodiment of the present invention is a method for producing furfural from a hemicellulose or xylose feedstock solution, comprising the steps of:
(1) taking the catalyst A prepared in example 1 into a glass pressure-resistant pipe, wherein the adding amount of the catalyst is 50% of the mass of the xylose substrate, and the proportion of an oil phase to a water phase is 4: 1, the xylose concentration was 0.5 kg/L.
(2) And (2) putting the glass pressure-resistant pipe in the system in the step (1) into an oil bath pot, heating to 160-190 ℃ under magnetic stirring, reacting for 60min, taking the upper oil phase and the lower water phase after the pressure-resistant pipe is cooled to room temperature, and detecting the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
The results were determined as shown in fig. 3, and the yields of furfural were 62.4%, 70.4%, 85.0%, and 76.5% when the reaction temperature was 160 ℃, 170 ℃, 180 ℃, and 190 ℃. When the reaction temperature is 180 ℃, the yield of the furfural is 85.0 percent at most.
Example 7
The sixth embodiment of the method for preparing furfural from hemicellulose or xylose raw material liquid comprises the following steps:
(1) taking the catalyst A prepared in example 1 into a glass pressure-resistant pipe, wherein the adding amount of the catalyst is 50% of the mass of the xylose substrate, and the proportion of an oil phase to a water phase is 4: 1, the xylose concentration is 0.5 kg/L.
(2) And (2) putting the glass pressure-resistant pipe in the system in the step (1) into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 40-120 min, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
According to the measurement, as shown in fig. 3, when the reaction time is 40min, 60min, 80min, 100min and 120min, the yield of furfural is 65.0%, 85.0%, 78.5%, 78.1% and 78.7%, respectively. When the reaction time is 60min, the yield of the furfural is up to 85.0%.
Example 8
The seventh embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) taking the catalyst A prepared in example 1 into a glass pressure-resistant pipe, wherein the adding amount of the catalyst is 50% of the mass of the xylose substrate, and the proportion of an oil phase to a water phase is 4: 1, the xylose concentration is 0.5 kg/L.
(2) Experiments were carried out using methyl isobutyl ketone, toluene, or tetrahydrofuran and its derivatives (e.g., 2-methyltetrahydrofuran, 2-ethyltetrahydrofuran, etc.), or benzylethyl ether, acetophenone, tetralin, etc., as the oil phase system of the reaction, respectively, according to the preferred ratio of the oil phase to the aqueous phase. Heating to 180 ℃ under magnetic stirring, reacting for 60min, after the reaction is finished, cooling the pressure-resistant pipe to room temperature, and taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
The determination result shows that the yield of furfural prepared by catalyzing xylose dehydration by different oil phase systems relative to the catalyst A is shown in the table 3.
TABLE 3 Effect of different oil phase systems on Furfural yield (xylose substrate)
As can be seen from table 3, the yield of furfural was up to 85.0% when methyl isobutyl ketone was used as the oil phase.
Example 9:
the eighth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) respectively weighing the catalysts A, B, C, D, E and F prepared in example 1 into a glass pressure resistant pipe, wherein the adding amount of the catalysts A, B, C, D, E and F is 50% of the mass of the hemicellulose substrate, and the proportion of an oil phase to a water phase is 4: 1, the concentration of hemicellulose is 0.25 kg/L.
(2) And (3) putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction solution obtained in the step (2), analyzing the furfural yield of the oil phase through a gas chromatograph, and analyzing the hemicellulose conversion rate of the water phase through a high performance liquid chromatograph with a differential detector.
The yield of furfural (Y) was determined when the amount of catalyst added was 50% of the mass of the substrateFF) As shown in table 4.
TABLE 4 influence of catalysts of different feed ratios on the yield of furfural (hemicellulose substrate)
| Serial number | A | B | C | D | E | F |
| YFF(％) | 75.3 | 70.1 | 64.2 | 66.5 | 61.9 | 57.7 |
As can be seen from Table 4, the yield Y of furfural was found when catalyst A was usedFFUp to 75.3%.
Example 10:
the ninth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) respectively weighing 10%, 15%, 20%, 25%, 30% g, 40%, 50%, 60%, 70% and 80% of catalyst A by mass of hemicellulose substrate, adding the catalyst A into a glass pressure-resistant pipe, wherein the ratio of oil phase to water phase is 4: 1, the concentration of hemicellulose is 0.25 kg/L.
(2) And (3) putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of hemicellulose by using a high performance liquid chromatograph with a differential detector for the water phase.
The determination result shows that the yield of furfural prepared by catalyzing hemicellulose to dehydrate by using the acidic ionic buffer solution catalyst A with different masses is shown in the table 5.
TABLE 5 influence of the amount of catalyst on the yield of furfural (hemicellulose substrate)
| Amount of |
10％ | 15％ | 20％ | 25％ | 30％ | 40％ | 50％ | 60％ | 70％ | 80％ |
| YFF(％) | 62.7 | 61.9 | 64.4 | 68.7 | 73.8 | 73.4 | 75.3 | 69.2 | 67.6 | 63.5 |
As is clear from Table 5, when catalysts A having different masses were used and the amount of the catalyst was 50%, the yield Y of furfural was found to beFFUp to 75.3%.
Example 11
The tenth embodiment of the method for preparing furfural from hemicellulose or xylose raw material liquid comprises the following steps:
(1) catalyst a prepared in example 1 was placed in a glass pressure tube, the ratio of oil phase to water phase was 4: 1, the adding amount of the catalyst is 50 percent of the mass of the substrate.
(2) Respectively weighing 0.15kg/L, 0.2kg/L, 0.25kg/L, 0.3kg/L, 0.35kg/L and 0.4kg/L of hemicellulose, adding into the system in the step (1), putting the glass pressure-resistant pipe into an oil bath pot, heating to 180 ℃ under magnetic stirring, reacting for 60min, after the reaction is finished, cooling the pressure-resistant pipe to room temperature, and taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of hemicellulose by using a high performance liquid chromatograph with a differential detector for the water phase.
As a result, as shown in the following table, when the hemicellulose concentrations were 0.15kg/L, 0.2kg/L, 0.25kg/L, 0.3kg/L, 0.35kg/L and 0.4kg/L, respectively, the furfural yields were as shown in Table 6.
TABLE 6 Effect of hemicellulose substrate concentration on Furfural yield (hemicellulose substrate)
| Concentration of hemicellulose (kg/L) | 0.15 | 0.2 | 0.25 | 0.3 | 0.35 | 0.4 |
| YFF(％) | 39.4 | 40.8 | 75.3 | 62.6 | 60.1 | 55.4 |
As can be seen from Table 5, the yield of furfural was 75.3% at a hemicellulose concentration of 0.25kg/L at the maximum.
Example 12:
the eleventh embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) the catalyst A prepared in example 1 was placed in a glass pressure tube, the hemicellulose concentration was 0.25kg/L, and the amount of catalyst added was 50% of the mass of the substrate.
(2) Respectively weighing the oil phase and the water phase in a ratio of 2: 1. 3: 1. 4: 1. 5: 1 and 6: 1, adding the mixture into the system in the step (1), placing a glass pressure-resistant pipe into an oil bath pan, heating the mixture to 180 ℃ under magnetic stirring, reacting for 60min, finishing the reaction, and after the pressure-resistant pipe is cooled to room temperature, taking an upper oil phase and a lower water phase to detect the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of hemicellulose by using a high performance liquid chromatograph with a differential detector for the water phase.
When the ratio of the oil phase to the water phase is determined to be 2: 1. 3: 1. 4: 1. 5: 1 and 6: at 1, the yields of furfural were 60.1%, 66.4%, 75.3%, 61.8%, and 53.6%, respectively. When the ratio of oil phase to water phase is 4: at 1, the yield of furfural was up to 75.3%.
Example 13:
the twelfth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) the catalyst A prepared in example 1 was placed in a glass pressure tube, the hemicellulose concentration was 0.25kg/L, the amount of catalyst added was 50% of the mass of the substrate, and the ratio of oil phase to water phase was 4: 1.
(2) and (2) putting the glass pressure-resistant pipe in the system in the step (1) into an oil bath pot, heating to 160-190 ℃ under magnetic stirring, reacting for 60min, taking the upper oil phase and the lower water phase after the pressure-resistant pipe is cooled to room temperature, and detecting the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of hemicellulose by using a high performance liquid chromatograph with a differential detector for the water phase.
The yields of furfural were determined to be 58.2%, 66.8%, 75.3%, and 70.2% when the reaction temperature was 160 ℃, 170 ℃, 180 ℃, and 190 ℃. When the reaction temperature is 180 ℃, the yield of the furfural is up to 75.3%.
Example 14
The thirteenth embodiment of the present invention for preparing furfural from hemicellulose or xylose feedstock solution comprises the following steps:
(1) taking the catalyst A prepared in example 1 into a glass pressure-resistant pipe, wherein the adding amount of the catalyst is 50% of the mass of the hemicellulose substrate, and the proportion of an oil phase to a water phase is 4: 1, the concentration of hemicellulose is 0.25 kg/L.
(2) And (2) putting the glass pressure-resistant tube in the system in the step (1) into an oil bath pan, heating to 180 ℃ under magnetic stirring, reacting for 40-120 min, after the reaction is finished, and after the pressure-resistant tube is cooled to room temperature, taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of hemicellulose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of hemicellulose by using a high performance liquid chromatograph with a differential detector for the water phase.
The yields of furfural were determined to be 62.1%, 75.3%, 71.2%, 73.4% and 73.6% when the reaction time was 40min, 60min, 80min, 100min and 120min, respectively. When the reaction time is 60min, the yield of the furfural is up to 75.3%.
Example 15
The fourteenth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
(1) taking the catalyst A prepared in example 1 into a glass pressure-resistant pipe, wherein the adding amount of the catalyst is 50% of the mass of the hemicellulose substrate, and the proportion of an oil phase to a water phase is 4: 1, the concentration of hemicellulose is 0.25 kg/L.
(2) Experiments were carried out using methyl isobutyl ketone, toluene, or tetrahydrofuran and its derivatives (e.g., 2-methyltetrahydrofuran, 2-ethyltetrahydrofuran, etc.), or benzylethyl ether, acetophenone, tetralin, etc., as the oil phase system of the reaction, respectively, according to the preferred ratio of the oil phase to the aqueous phase. Heating to 180 ℃ under magnetic stirring, reacting for 60min, after the reaction is finished, cooling the pressure-resistant pipe to room temperature, and taking the upper oil phase and the lower water phase to detect the yield of furfural and the conversion rate of xylose.
(3) And (3) taking the oil phase and water phase reaction liquid obtained in the step (2), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
Through determination, the yield of different oil phase systems for preparing furfural by catalyzing the dehydration of hemicellulose by using the acidic ion buffer solution catalyst A is shown in table 7.
TABLE 7 influence of different oil phase systems on the yield of furfural (hemicellulose as substrate)
As can be seen from table 7, the yield of furfural was up to 75.3% when methyl isobutyl ketone was used as the oil phase.
Example 16
With reference to fig. 1, the system for preparing furfural from hemicellulose or xylose feedstock according to the present invention can be used to produce furfural products, and different furfural yields can be achieved by adjusting the parameters of the equipment. In addition, the water phase, the oil phase and the acidic ion buffer solution catalyst can be recycled in the whole furfural production process.
The specific process flow for realizing the annual production of the furfural reaches 2000 tons is as follows, and the annual production time is 300 days. The raw material liquid (with the concentration of 0.25kg/L) and the acidic ionic buffer solution catalyst (50 percent of the substrate mass) are uniformly mixed by a static mixer 1 at the flow rates of 370kg/h and 100kg/h respectively to obtain mixed material liquid, the mixed material liquid enters a reaction extraction tower 2, and simultaneously, an oil phase solution is added from the bottom of the reaction extraction tower 2 at the flow rate of 1480 kg/h. Heating the reaction extraction tower 2 to 175-185 ℃, reacting and staying for 50-70 min, extracting oil phase gas containing furfural from an oil phase outlet 22 at the top of the reaction extraction tower 2, and respectively reaching a second rectifying tower system 4 through a second valve 9 (when the boiling point of the used oil phase is lower than the boiling point of furfural), or reaching a first rectifying tower system 3 through a first valve 8 (when the boiling point of the used oil phase is higher than the boiling point of furfural) for rectification and purification to obtain a furfural product. The oil phase in the first rectifying tower system 3 and the oil phase in the second rectifying tower system 4 are processed by the filtering device and then return to the reactive extraction tower 2 for recycling, and participate in the next extraction process.
The specific process flow for realizing the annual production of the furfural of 5000 tons is as follows, and the annual production time is 300 days. The raw material liquid (with the concentration of 0.25kg/L) and the acidic ionic buffer solution catalyst (50 percent of the substrate mass) are uniformly mixed by a static mixer 1 at the flow rates of 922kg/h and 232kg/h respectively to obtain mixed material liquid, the mixed material liquid enters a reaction extraction tower 2, and simultaneously, an oil phase solution is added from the bottom of the reaction extraction tower 2 at the flow rate of 3690 kg/h. Heating the reaction extraction tower 2 to 175-185 ℃, reacting and staying for 50-70 min, pumping out oil phase gas containing furfural from a tower top oil phase outlet 22 of the reaction extraction tower 2, and respectively reaching a second rectification tower system 4 through a second valve 9 (when the boiling point of the used oil phase is lower than the boiling point of furfural) or reaching a first rectification tower system 3 through a first valve 8 (when the boiling point of the used oil phase is higher than the boiling point of furfural) for rectification and purification to obtain a furfural product. The oil phase in the first rectifying tower system 3 and the oil phase in the second rectifying tower system 4 are processed by the filtering device and then return to the reactive extraction tower 2 for recycling, and participate in the next extraction process.
Example 17
The fifteenth embodiment of the method for preparing furfural from hemicellulose or xylose raw material liquid comprises the following steps:
in the process described in example 16, we studied the production process of different oil phases with boiling points lower than that of furfural (such as methyl isobutyl ketone, toluene, or tetrahydrofuran, 2-methyltetrahydrofuran, 2-ethyltetrahydrofuran, etc.) with an annual yield of 2000 tons, and the specific implementation method is as follows: the raw material liquid (concentration 0.25kg/L) and the acidic ionic buffer solution catalyst (50% of the substrate mass) were uniformly mixed by the static mixer 1 at flow rates of 370kg/h and 100kg/h, respectively, into the reactive extraction column 2, while the oil phase solution was fed from the bottom of the reactive extraction column 2 at a flow rate of 1480 kg/h. Heating the reaction extraction tower 2 to 175-185 ℃, reacting and staying for 50-70 min, extracting oil phase gas containing furfural from an oil phase outlet 22 at the top of the reaction extraction tower 2, and respectively reaching a second rectifying tower system 4 through a second valve 9 for rectification and purification to obtain a furfural product. The oil phase in the second rectifying tower system 4 is processed by the filtering device and then returns to the reactive extraction tower 2 for recycling, and participates in the next extraction process.
Example 18
The sixteenth embodiment of the method for preparing furfural by using hemicellulose or xylose raw material liquid comprises the following steps:
aiming at the process flow described in embodiment 16, taking an annual output of 2000 tons as an example, we studied the production flow when different oil phases with boiling points higher than that of furfural are used as solvents (such as benzyl ethyl ether, acetophenone, tetralin, etc.), and the specific implementation method is as follows: the raw material liquid (concentration 0.25kg/L) and the acidic ionic buffer solution catalyst (50% of the substrate mass) were uniformly mixed by the static mixer 1 at flow rates of 370kg/h and 100kg/h, respectively, into the reactive extraction column 2, while the oil phase solution was fed from the bottom of the reactive extraction column 2 at a flow rate of 1480 kg/h. Heating the reaction extraction tower 2 to 175-185 ℃, reacting and staying for a period of 50-70 min, pumping oil phase gas containing furfural out of a tower top oil phase outlet 22 of the reaction extraction tower 2, respectively passing through a first valve 8, and reaching a first rectifying tower system 3 (when the boiling point of the used oil phase is higher than that of furfural), and rectifying and purifying to obtain a furfural product. The oil phase in the first rectifying tower system 3 is processed by the filtering device and then returns to the reactive extraction tower 2 for recycling, and participates in the next extraction process.
Example 19
The seventeenth embodiment of the present invention, which is a method for producing furfural using hemicellulose or xylose feedstock solution, comprises the steps of:
(1) aiming at the process flow described in the embodiment 16, taking the annual output of 2000 tons as an example, we study the cyclic usability of the catalyst and the oil phase system, and the specific implementation method is as follows: the raw material liquid (concentration 0.25kg/L) and the catalyst A (50% of the substrate mass) were uniformly mixed by the static mixer 1 at flow rates of 370kg/h and 100kg/h, respectively, into the reactive extraction column 2, while the oil phase solution was fed from the bottom of the reactive extraction column 2 at a flow rate of 1480 kg/h. Methyl isobutyl ketone was used as the oil phase. Heating the reaction extraction tower 2 to 175-185 ℃, reacting and staying for a period of 50-70 min, pumping out oil phase gas containing furfural from an oil phase outlet 22 at the top of the reaction extraction tower 2, respectively passing through a first valve 8, and reaching a first rectifying tower system 3 (when the boiling point of the used oil phase is higher than that of furfural), and rectifying and purifying to obtain a furfural product. In order to explore the recycling performance of the catalyst and the oil phase system, the oil phase and the catalyst A in the first rectifying tower system 3 sequentially pass through a filtering and adsorbing device and then return to the reactive extraction tower 2 for the next recycling experiment, and the process is repeated for multiple times.
(2) And (2) taking the oil phase and water phase reaction liquid obtained in the step (1), analyzing the yield of furfural by using a gas chromatograph, and analyzing the conversion rate of xylose by using a high performance liquid chromatograph with a differential detector for the water phase.
The specific recycling properties of catalyst a and the methyl isobutyl ketone oil phase system were determined as shown in tables 8 and 9:
TABLE 8 circulation performance of catalyst A (hemicellulose as substrate)
| Number of |
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| YFF(％) | 75.0 | 74.2 | 75.4 | 75.6 | 75.1 | 75.8 | 74.9 | 76.2 | 76.0 | 74.5 |
TABLE 9 circulation behaviour of methyl isobutyl ketone oil phase system (hemicellulose as substrate)
| Number of |
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| YFF(％) | 75.0 | 75.3 | 74.7 | 74.2 | 74.0 | 74.9 | 75.5 | 75.1 | 75.3.0 | 74.8 |
As can be seen from tables 8 and 9, after the catalyst a and the methylisobutylketone oil phase system were used repeatedly (10 times), there was little sign of reduction in the size of furfural yield, indicating that the stability of the catalyst a was good and the stability of the oil phase was also good.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the utility model, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the utility model.
Claims (7)
1. A system for preparing furfural by utilizing hemicellulose or xylose raw material liquid is characterized by comprising a static mixer, a reaction extraction tower and a rectification tower system, wherein the rectification tower system is used for separating a furfural component from an oil phase extracting agent in the oil phase extracting agent containing the furfural component, the static mixer is respectively provided with a hemicellulose or xylose raw material liquid feeding port, a catalyst feeding port and a mixed liquid discharging port, the mixed liquid discharging port is communicated with a feeding port at the upper part of the reaction extraction tower through a water phase pipeline, the upper part of the reaction extraction tower is also provided with an oil phase outlet convenient for the oil phase extracting agent containing the furfural component in the reaction extraction tower to leave, the bottom of the reaction extraction tower is provided with an oil phase inlet convenient for the oil phase extracting agent to enter the reaction extraction tower, and an oil phase input pipeline is communicated with the oil phase inlet; the oil phase outlet is communicated with the feed end of the rectifying tower system through a pipeline, and a furfural collecting pipeline is arranged on the rectifying tower system and used for collecting furfural products.
2. The system for preparing furfural by using hemicellulose or xylose raw material liquid according to claim 1, wherein the rectifying tower system comprises a first rectifying tower and a second rectifying tower, the first rectifying tower is communicated with the oil phase outlet through a first pipeline, the second rectifying tower is communicated with the oil phase outlet through a second pipeline, and furfural collecting pipelines are respectively arranged at the bottom of the second rectifying tower system or at the top of the first rectifying tower system and used for collecting furfural products.
3. The system for producing furfural using a hemicellulose or xylose feedstock as claimed in claim 2, wherein a first collecting port for recovering the oil phase extractant is provided at the bottom of the first distillation column system, a second collecting port for recovering the oil phase extractant is provided at the bottom of the second distillation column system, the first collecting port is connected to the oil phase inlet port via a first oil phase recovery line, the second collecting port is also connected to the oil phase inlet port via a second oil phase recovery line, and the first oil phase recovery line is provided with a second filter and a second adsorber for removing impurities in the recovered oil phase extractant.
4. The system for producing furfural using hemicellulose or xylose feedstock liquid according to claim 2, wherein the first pipeline and the second pipeline are respectively communicated with an oil phase outlet through return pipelines, and an oil phase pump is provided on the return pipelines.
5. The system for preparing furfural from hemicellulose or xylose raw material liquid according to claim 1 or 2, further comprising an evaporation system, wherein a water phase outlet is further arranged at the bottom of the reactive extraction tower, the water phase outlet is communicated with a feeding end of the evaporation system through a discharge pipeline, a water vapor discharge port and a concentrated liquid discharge port are further arranged on the evaporation system, the concentrated liquid discharge port is communicated with a feeding port of the static mixer through a concentrated liquid pipeline, and a first filter and a first adsorber for removing impurities in the concentrated liquid are respectively arranged on the concentrated liquid pipeline.
6. The system for producing furfural using a hemicellulose or xylose feedstock liquid according to claim 5, wherein a discharge pump is provided on the discharge conduit.
7. The system for producing furfural from a hemicellulose or xylose feedstock liquid according to claim 5, wherein a first concentration pump is provided on the concentrate line between the concentrate discharge port and the first filter, and a second concentration pump is provided on the concentrate line between the first adsorber and the feed port of the static mixer.
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| CN114345376B (en) * | 2022-01-07 | 2024-08-09 | 浙江华康药业股份有限公司 | Acidic ion buffer catalyst, preparation method thereof, and system and method for preparing furfural by using catalyst |
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