CN109232774B - Method for separating and purifying hemicellulose in prehydrolysis liquid in dissolving pulp pretreatment working section - Google Patents
Method for separating and purifying hemicellulose in prehydrolysis liquid in dissolving pulp pretreatment working section Download PDFInfo
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- 229920002488 Hemicellulose Polymers 0.000 title claims abstract description 41
- 239000007788 liquid Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002244 precipitate Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000002023 wood Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 229920000831 ionic polymer Polymers 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000008399 tap water Substances 0.000 claims description 2
- 235000020679 tap water Nutrition 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004537 pulping Methods 0.000 abstract description 2
- 241000220479 Acacia Species 0.000 description 6
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 230000003113 alkalizing effect Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 102100030386 Granzyme A Human genes 0.000 description 1
- 101001009599 Homo sapiens Granzyme A Proteins 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a method for separating and purifying hemicellulose in prehydrolysis liquid in a dissolving pulp pretreatment working section, and belongs to the field of pulping and papermaking. The method comprises the following steps: firstly, wood chips and water are kept at the temperature of 150-; acidifying the supernatant II with acid to pH 1.5-2.5, and centrifuging to obtain supernatant III; mixing the supernatant III with the non-ionic polymer, and centrifuging to obtain a supernatant IV; alkalifying the supernatant IV with alkali to a pH value of 6-10, centrifuging to obtain a supernatant V, mixing the supernatant V with ethanol, standing, collecting precipitate, and drying to obtain hemicellulose. The method has the advantages of high purity of the obtained hemicellulose, simple operation, low cost, environmental protection and the like.
Description
Technical Field
The invention relates to a method for separating and purifying hemicellulose in prehydrolysis liquid in a dissolving pulp pretreatment working section, and belongs to the field of pulping and papermaking.
Background
The pretreatment of plant fiber raw materials in the production of dissolving pulp is a widely used method. The specific implementation is that the self-hydrolysis of the plant fiber raw material is carried out under certain temperature conditions, and a large amount of hemicellulose and partial lignin are dissolved out, so as to be beneficial to subsequent chemical cooking. In the process, the prehydrolysis liquid is usually mixed with black liquor as waste liquid and sent to a soda recovery furnace for combustion, and the additional value of the combustion treatment method is low, so that the waste of biomass resources is caused. Today, environmental protection and resource conservation are advocated, and effective utilization of prehydrolysis liquid needs to be explored.
For the degree of pretreatment, P factor is generally adopted for characterization, the P factor is proposed by Brash et al in the sixty-seven years of the last century and is similar to the concept of cooking H factor, so that two factors of prehydrolysis temperature and time are integrated into one variable, Sixta et al further illustrate the concept of P factor and provide a calculation formula of P factor on the basis of carbohydrate glycosidic bond fracture activation energy for guiding the preparation of prehydrolysis process conditions, and the higher the P factor is, the deeper the degree of pretreatment is.
If the heating rate is constant, the calculation can be carried out according to the Simpson expansion, and the total P factor is the sum of the P factors in the heating stage and the heat preservation stage. The P factor is calculated as follows:
wherein: t is0-initial temperature, K; t-temperature at any time, K; t-by T0And (4) heating to T for required time h.
With the pre-hydrolysis process, the hemicellulose in the pre-hydrolysis liquid can be gradually converted into products such as formic acid, acetic acid, furfural and the like.
Disclosure of Invention
The invention solves the problems by concentrating, acidifying, flocculating non-ionic high polymer, alkalizing, separating and purifying hemicellulose in the prehydrolysis liquid.
The invention provides a method for separating and purifying hemicellulose in prehydrolysis liquid in a dissolving pulp pretreatment workshop section, which comprises the following steps: firstly, wood chips and water are kept at the temperature of 150-; acidifying the supernatant II with acid to pH 1.5-2.5, and centrifuging to obtain supernatant III; mixing the supernatant III with the non-ionic polymer, and centrifuging to obtain a supernatant IV; alkalifying the supernatant IV with alkali to a pH value of 6-10, centrifuging to obtain a supernatant V, mixing the supernatant V with ethanol, standing, collecting precipitate, and drying to obtain hemicellulose.
The invention preferably has a weight ratio of wood chips to water of 1: 3-8.
The present invention preferably provides that the concentration is 30-90% by volume.
The acid is preferably concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or acetic acid.
In the invention, the nonionic polymer is preferably polyethylene oxide or polyethylene glycol.
Preferably, the alkali is sodium hydroxide, potassium hydroxide, calcium hydroxide or barium hydroxide.
The volume ratio of the supernatant V to the ethanol is preferably 1: 4-10.
The invention preferably has the standing time of 0.5-2 h.
The invention has the beneficial effects that:
the method has the advantages of high purity of the obtained hemicellulose, simple operation, low cost, environmental protection and the like.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
The origin of the acacia wood is vietnam, and the water content of the acacia wood is 6%.
Example 1
Preparing prehydrolysis liquid:
106.4g of acacia wood chips (corresponding to 100g of absolute acacia wood chips) were taken and the weight ratio of 1: 4 liquid ratio and tap water are prehydrolyzed, the temperature is raised to 170 ℃, different heat preservation times are set to obtain the prehydrolysis liquid with the expected P factors, the P factors are respectively 100, 130, 160, 200, 250, 300, 500, 700, 900 and 1100, after heat preservation is finished, cooling and centrifugation are carried out, supernatant is collected, and the components of the acacia senii prehydrolysis liquid are shown in the following table 1.
TABLE 1 ingredients of acacia prehydrolysis liquid
| P factor | 100 | 130 | 160 | 200 | 250 | 300 | 500 | 700 | 900 | 1100 |
| pH | 3.57 | 3.23 | 3.18 | 3.15 | 3.13 | 3.11 | 3.07 | 3.07 | 3.05 | 3.03 |
| Solids content/% | 0.62 | 1.38 | 1.52 | 1.64 | 1.77 | 2.38 | 2.62 | 2.81 | 3.01 | 3.33 |
| Ash content% | 0.027 | 0.036 | 0.032 | 0.035 | 0.043 | 0.046 | 0.051 | 0.053 | 0.050 | 0.058 |
| Lignin content g/L | 2.41 | 2.80 | 3.13 | 3.65 | 3.82 | 4.00 | 4.19 | 4.35 | 5.28 | 5.44 |
| Xylose content g/L | 1.11 | 4.34 | 6.17 | 9.22 | 10.80 | 12.29 | 14.31 | 18.31 | 18.50 | 17.07 |
Example 2
Determining the optimal P factor condition of prehydrolysis:
taking 100mL of prehydrolysis liquid of different P factors respectively, and mixing the prehydrolysis liquid according to the ratio of 1: mixing the mixture with ethanol in a volume ratio of 6, standing for 1h, collecting precipitate, drying, and obtaining the quality and purity of the hemicellulose precipitate shown in the following table 2.
TABLE 2 quality and purity of hemicellulose precipitate
| P factor | 100 | 130 | 160 | 200 | 250 | 300 | 500 | 700 | 900 | 1100 |
| Mass g/L | 1.42 | 2.45 | 2.86 | 2.94 | 2.31 | 2.10 | 0.50 | 0.37 | 0.26 | 0.21 |
| Purity% | 65.5 | 70.1 | 69.9 | 71.2 | 66.6 | 70.0 | 53.9 | 29.0 | — | — |
From table 2, P factor 200 is the optimal prehydrolysis condition.
Example 3
Determining the optimal volume ratio of the prehydrolysis liquid to the ethanol:
taking 100mL of prehydrolysis liquid with P factor of 200, and respectively carrying out hydrolysis according to the weight ratio of 1: 4. 1: 6. 1: 8. 1: 10 and 1: mixing the mixture with ethanol in a volume ratio of 12, standing for 1h, collecting precipitate, drying, and obtaining the quality and purity of the hemicellulose precipitate shown in the following table 3.
TABLE 3 quality and purity of hemicellulose precipitate
| Volume ratio of | 1：4 | 1：6 | 1：8 | 1：10 | 1:12 |
| Mass g/L | 1.66 | 2.94 | 3.43 | 3.61 | 3.66 |
| Purity% | 72.6 | 71.2 | 70.7 | 69.6 | 74.6 |
From table 3, the mass of the collected hemicellulose is gradually increased with the increase of the volume ratio, but the increasing trend is gradually reduced, and the purity of the collected hemicellulose is not obviously changed, and the volume ratio is 1: 8. 1: 10 and 1: 12 ratio, in consideration of economy, the volume ratio of prehydrolysis liquid to ethanol is 1: and 8 is the optimal volume ratio.
Example 4
Determining an optimal concentration volume fraction:
taking 100mL of prehydrolysis liquid with P factor of 200, concentrating the prehydrolysis liquid with the volume fractions of 10%, 30%, 50%, 70% and 90%, respectively, centrifuging to obtain supernatant, and mixing the supernatant according to the ratio of 1: mixing the supernatant with ethanol at a volume ratio of 8, standing for 1h, collecting the precipitate, drying, and obtaining the quality and purity of the hemicellulose precipitate shown in the following table 4.
TABLE 4 quality and purity of hemicellulose precipitate
| Fractional volume of concentration | 10％ | 30％ | 50％ | 70％ | 90％ |
| Mass g/L | 3.70 | 4.78 | 5.45 | 5.90 | 6.11 |
| Purity% | 69.1 | 72.3 | 69.2 | 72.8 | 71.4 |
From table 4, the mass of the collected hemicellulose precipitates gradually increased with the increase of the concentration volume fraction, while the purity of the collected hemicellulose precipitates was not significantly changed, but the unit amount of ethanol was decreased, so 90% was the optimal concentration volume fraction.
Example 5
Determining optimal acidification:
acidifying the prehydrolysis liquid with the P factor of 200 and the concentration of 90% by using concentrated sulfuric acid until the prehydrolysis liquid is respectively acidified to 3.0, 2.5, 2.0 and 1.5, centrifuging to obtain a supernatant, and mixing the supernatant with the concentrated sulfuric acid according to the ratio of 1: mixing the supernatant with ethanol at a volume ratio of 8, standing for 1h, collecting the hemicellulose precipitate, and drying, wherein the quality and purity of the hemicellulose precipitate are shown in Table 5 below.
TABLE 5 quality and purity of hemicellulose precipitate
| pH | 3 | 2.5 | 2 | 1.5 |
| Mass g/L | 6.06 | 5.95 | 5.43 | 5.37 |
| Purity% | 75.2 | 76.0 | 79.2 | 79.4 |
As can be seen from Table 5, the quality of the collected hemicellulose was decreased as the pH was decreased, but the purity of the collected hemicellulose was gradually increased, and the absolute amount of the sugar components therein was not significantly changed, so that pH 2.0 was the optimum acidic environment.
Example 6
Flocculation treatment of non-ionic polymer:
adding a polyoxyethylene solution with the mass fraction of 5% into prehydrolysis liquid which is concentrated by 90% and acidified to the pH value of 2 and has the P factor of 200 to ensure that the mass concentration of the prehydrolysis liquid is 200mg/L, stirring for 10min, centrifuging, and mixing supernatant with ethanol in a volume ratio of 1: 8, mixing, standing for 1h, collecting hemicellulose precipitate, drying, and detecting that 5.26g of hemicellulose can be collected per liter of prehydrolysis liquid, wherein the purity of the hemicellulose can reach 87%.
Example 7
Determining the optimal alkalization:
respectively alkalizing prehydrolysis liquid which is subjected to P factor 200, concentration of 90%, acidification to pH value of 2 and flocculation treatment of 200mg/L polyoxyethylene by using 50% by mass of sodium hydroxide solution, respectively alkalizing to 4.0, 6.0, 8.0, 10.0 and 12.0, centrifuging to obtain supernate, and mixing the supernate according to the weight ratio of 1: mixing the supernatant with ethanol at a volume ratio of 8, standing for 1h, collecting the hemicellulose precipitate, and drying, wherein the quality and purity of the hemicellulose precipitate are shown in Table 6 below.
TABLE 6 quality and purity of hemicellulose precipitate
| pH | 4 | 6 | 8 | 10 | 12 |
| Mass g/L | 7.44 | 9.87 | 9.94 | 10.35 | 12.74 |
| Purity% | 78.2 | 76.4 | 75.8 | 73.1 | 69.9 |
| Ash content% | 8.0 | 9.1 | 9.0 | 9.3 | 20.1 |
From table 6, the quality of the collected hemicellulose precipitate gradually increases with the increase of the pH value, but the purity of the collected hemicellulose precipitate gradually decreases, the yield and purity of the hemicellulose precipitate are comprehensively considered, and the pH value of 8 is an optimal alkaline environment.
Claims (4)
1. A method for separating and purifying hemicellulose in prehydrolysis liquid in a dissolving pulp pretreatment workshop section is characterized by comprising the following steps: the method comprises the following steps:
firstly, wood chips and water are insulated at the temperature of 170 ℃ until the P factor is 200, and the weight ratio of the wood chips to tap water is 1: 4, cooling, centrifuging to obtain a supernatant I, concentrating, wherein the volume percentage of the concentration is 90%, and centrifuging to obtain a supernatant II; acidifying the supernatant II with acid until the pH is 2, and centrifuging to obtain a supernatant III;
mixing the supernatant III with a non-ionic polymer, wherein the non-ionic polymer is polyoxyethylene, and centrifuging to obtain a supernatant IV;
alkalifying the supernatant IV by using alkali to the pH value of 8, centrifuging to obtain a supernatant V, and mixing the supernatant V with ethanol uniformly, wherein the volume ratio of the supernatant V to the ethanol is 1: and 8, standing, collecting the precipitate, and drying to obtain the hemicellulose.
2. The method for separating and purifying hemicellulose in prehydrolysis liquid in the dissolving pulp pretreatment workshop section according to claim 1, is characterized in that: the acid is concentrated sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid or acetic acid.
3. The method for separating and purifying hemicellulose in prehydrolysis liquid in the dissolving pulp pretreatment workshop section according to claim 2, characterized in that: the alkali is sodium hydroxide, potassium hydroxide, calcium hydroxide or barium hydroxide.
4. The method for separating and purifying hemicellulose in prehydrolysis liquid in the dissolving pulp pretreatment workshop section according to claim 3, characterized in that: the standing time is 0.5-2 h.
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| SE1950785A1 (en) * | 2019-06-26 | 2020-11-03 | Valmet Oy | Method for extracting hemicellulose from lignocellulosic material |
| CN110295510B (en) * | 2019-06-27 | 2021-10-01 | 大连工业大学 | Method for preparing lignin crude product and sugar solution by using pulping and papermaking waste liquor |
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