CN113564956B - Prehydrolysis method for improving delignification efficiency of grape branches by sulfate process - Google Patents

Prehydrolysis method for improving delignification efficiency of grape branches by sulfate process Download PDF

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CN113564956B
CN113564956B CN202110791842.3A CN202110791842A CN113564956B CN 113564956 B CN113564956 B CN 113564956B CN 202110791842 A CN202110791842 A CN 202110791842A CN 113564956 B CN113564956 B CN 113564956B
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grape
heteropoly acid
branches
acid
grape branches
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CN113564956A (en
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李涛
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Shaanxi Institute of Technology
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C1/00—Pretreatment of the finely-divided materials before digesting
    • D21C1/04—Pretreatment of the finely-divided materials before digesting with acid reacting compounds
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
    • D21H11/04—Kraft or sulfate pulp
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Abstract

The invention discloses a prehydrolysis method for improving delignification efficiency of grape branches by a sulfate method. The method utilizes the recyclable heteropoly acid to improve the prehydrolysis effect, increases the delignification efficiency in the sulfate cooking process, and prepares the high-quality chemical pulp. Meanwhile, the invention utilizes grape branches which are one of agricultural and forestry wastes to realize resource utilization, increases the source of chemical pulp raw materials and has the characteristic of environmental friendliness.

Description

Prehydrolysis method for improving delignification efficiency of grape branches by sulfate process
Technical Field
The invention belongs to the fields of applied chemistry and pulping and papermaking engineering, and particularly relates to a method for improving delignification efficiency of a grape branch sulfate method by using a heteropoly acid reinforced prehydrolysis process.
Background
As the most classical cooking method, the sulfate pulping method has the advantages of wide raw material adaptability, high pulping strength and the like; but also has the defects of high chemical price, low yield and the like. The pre-hydrolysis before cooking can effectively reduce the delignification pressure of the cooking section, thereby obtaining higher economic benefit. The dilute acid prehydrolysis has been widely paid attention and applied once for the reason that the dilute acid prehydrolysis has better economical efficiency and high efficiency, but the equipment corrosion and the acid recovery caused by the dilute acid prehydrolysis are bottlenecks which disturb the further development of the acid prehydrolysis. Compared with dilute acid prehydrolysis, hot water prehydrolysis has the advantages of single reaction medium, low energy consumption, less pollution and the like, but because of the lack of acid addition, the dissociation of cellulose and hemicellulose is limited. Clearly, how to achieve or even exceed the desired effect of prehydrolysis; it is important to overcome the problems of acid recovery and equipment corrosion.
Disclosure of Invention
The invention aims to provide a prehydrolysis method for improving delignification efficiency of grape branches by a sulfate method, so as to overcome the problems in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a prehydrolysis method for improving delignification efficiency of grape branches by a sulfate method comprises the following steps:
(1) pruning grape branches, peeling off the skins of the grape branches, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the grape branches treated in the step (1) into a mixed solution with the solid content of 0.1-10% by using a heteropoly acid aqueous solution, and soaking the mixed solution to ensure that the heteropoly acid is fully contacted with the grape branches to obtain a grape branch/heteropoly acid suspension;
(3) treating the grape branch/heteropoly acid suspension prepared in the step (2) at 110-180 ℃ for 2-60 minutes to ensure that the grape branch/heteropoly acid suspension fully reacts to obtain a mixture containing grape branch fibers and heteropoly acid solution;
(4) carrying out solid-liquid separation on the mixture obtained in the step (3), washing the mixture to be neutral by using clear water, and then cooking the mixture by using a sulfate method; and after the steaming and boiling are finished, carrying out solid-liquid separation, washing with clear water to be neutral, and drying to finally obtain the grape branch chemical pulp.
Further, pruning the grape branches to a length of 2-3cm in step (1).
Further, in the step (1), the content of holocellulose in the grape branches is 40-80%, and the balance is the Clarsen lignin and ash.
Further, the heteropoly acid in the step (2) is one or a mixture of more of phosphotungstic acid, silicotungstic acid and silicomolybdic acid.
Further, the concentration of the heteropoly acid aqueous solution in the step (2) is 0.001-0.1 mol/L.
Further, the soaking time in the step (2) is 0.2-120 h.
Further, the cooking conditions in the step (4) are effective alkali: 16% by weight of Na 2 O meter, degree of vulcanization: 18% by weight of Na 2 And (3) measuring the ratio of O to solid to liquid, wherein the cooking temperature is 140 ℃, and the heat preservation time is 40 min.
Further, in the step (4), after the mixture was subjected to solid-liquid separation, the heteropoly acid in the liquid phase was recovered by ether extraction.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention uses grape branches which are one of agricultural and forestry wastes as raw materials, and can reduce the risk of burning the grape branches while fully utilizing the effective components of the grape branches. Meanwhile, the invention adopts the prehydrolysis treatment of heteropoly acid, and utilizes the strong acidity of heteropoly acid to dissolve out most of hemicellulose in the raw material, thereby effectively reducing the subsequent cooking pressure. The grape branches which are prehydrolyzed by heteropoly acid can be cooked into pulp under the condition of light cooking.
The heteropolyacid adopted by the invention is a class of oxygen-containing polyacid which is formed by coordination and bridging of heteroatoms (such as P, Si and the like) and polyatomic atoms (such as Mo, W and the like) through oxygen atoms according to a certain structure, and has high catalytic activity, strong acidity and good stability. The heteropoly acid adopted by the invention is soluble in water, can be completely ionized in water and is easy to recover, so that a large amount of hydrogen ions exist in the aqueous solution of the heteropoly acid and can be used for acid prehydrolysis. Meanwhile, the catalytic action of the heteropoly acid can promote the degradation of lignin and improve the dissolution rate of the lignin in the subsequent cooking process.
In addition, a large amount of hydrogen protons in the heteropoly-acid can freely interact with oxygen atoms in various chemical bonds, so the heteropoly-acid can be recovered by methods such as ether extraction, ethanol precipitation and the like, and the prehydrolysis effect after recovery is almost unchanged, so the heteropoly-acid has environmental friendliness and good economic benefit.
Detailed Description
The invention is further described below.
A prehydrolysis method for improving delignification efficiency of grape branches by a sulfate method mainly comprises the steps of material preparation, heteropoly acid prehydrolysis and sulfate method cooking. The method utilizes the recyclable heteropoly acid to improve the prehydrolysis effect, increases the delignification efficiency in the sulfate cooking process, and prepares the high-quality chemical pulp. Meanwhile, the invention utilizes grape branches which are one of agricultural and forestry wastes to realize resource utilization, increases the source of chemical pulp raw materials and has the characteristic of environmental friendliness.
The method comprises the following specific steps:
(1) pruning grape branches to 2-3cm length, peeling off the skin, sealing and storing at room temperature, and balancing water for later use; wherein, the content of the holocellulose is 40 percent to 80 percent, and the rest is the Clarsen lignin and ash content;
(2) preparing the treated grape branches into 0.1-10% of solid content by using 0.001-0.1mol/L heteropoly acid aqueous solution, and soaking for 0.2-120h to ensure that the heteropoly acid is fully contacted with the grape branches; wherein the heteropoly acid is one or a mixture of more of phosphotungstic acid, silicotungstic acid and silicomolybdic acid;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating for 2-60 minutes at 110-180 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing grape branch fibers pretreated by heteropoly acid;
(4) mixing the above materialsSeparating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
(1) Pruning grape branches with the holocellulose content of 79.80% to have the length of 2-3cm, peeling off the skins, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the treated grape branches into 0.1% solid content by using 0.001mol/L phosphotungstic acid aqueous solution, and soaking for 0.2h to ensure that the phosphotungstic acid is fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating for 60 minutes at 110 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing grape branch fibers pretreated by heteropoly acid;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The yield of the grape branch chemical pulp obtained in the example is 35.05 percent, and the alpha-fiberThe content of the element is 91.03 percent, and the alkali solubility is S 10 And S 18 7.25% and 5.93%, respectively, and a kappa number of 5.54.
Example 2
(1) Pruning grape branches with the holocellulose content of 73.53 percent to have the length of 2-3cm, peeling off the skins, sealing and storing at room temperature, and balancing the water for later use;
(2) preparing the treated grape branches into 0.25% solid content by using silicotungstic acid aqueous solution with the concentration of 0.005mol/L, and soaking for 1h to ensure that the silicotungstic acid is fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution for 50 minutes at 120 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing grape branch fibers pretreated by heteropoly acid;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The grape branch chemical pulp obtained in the example has the yield of 34.83 percent, the content of alpha-cellulose of 89.95 percent and the alkali solubility S 10 And S 18 8.73% and 6.55%, respectively, and a kappa number of 6.05.
Example 3
(1) Pruning grape branches with the holocellulose content of 64.95% to be 2-3cm long, peeling off the skins, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the treated grape branches into 0.5% solid content by using silicomolybdic acid aqueous solution with the concentration of 0.01mol/L, and soaking for 5 hours to ensure that the silicomolybdic acid is fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution at 130 ℃ for 40 minutes to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing the grape branch fibers pretreated by heteropoly acid;
(4) solidifying the mixtureSeparating liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The grape branch chemical pulp obtained in this example has a yield of 36.83%, an alpha-cellulose content of 92.55%, and an alkali solubility S 10 And S 18 4.15% and 2.83%, respectively, and a kappa number of 5.98.
Example 4
(1) Pruning grape branches with the holocellulose content of 59.94% to have the length of 2-3cm, peeling off the skins, sealing and storing at room temperature, and balancing the water for later use;
(2) preparing the treated grape branches into 1% solid content by using a mixed aqueous solution of phosphotungstic acid and silicotungstic acid with the concentration of 0.025mol/L, and soaking for 20 hours to ensure that the phosphotungstic acid and silicotungstic acid are fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution for 30 minutes at 140 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing heteropoly acid pretreated grape branch fibers;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The grape branch chemical pulp obtained in this example has a yield of 33.95%, an alpha-cellulose content of 92.15%, and an alkali solubility S 10 And S 18 6.33% and 4.53%, respectively, and a kappa number of 6.31.
Example 5
(1) Pruning grape branches with the holocellulose content of 52.98% to have the length of 2-3cm, peeling off the skins, sealing and storing at room temperature, and balancing the water for later use;
(2) preparing the treated grape branches into 2% solid content by using a mixed aqueous solution of silicomolybdic acid and silicotungstic acid with the concentration of 0.05mol/L, and soaking for 40 hours to ensure that the silicomolybdic acid and the silicotungstic acid are fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution for 20 minutes at 150 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing heteropoly acid pretreated grape branch fibers;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The grape branch chemical pulp obtained in the example has the yield of 29.93 percent, the content of alpha-cellulose of 93.88 percent and the alkali solubility S 10 And S 18 6.14% and 4.03%, respectively, and a kappa number of 4.95.
Example 6
(1) Pruning grape branches with 45.08 percent of holocellulose to be 2-3cm long, peeling off the skins of the grape branches, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the treated grape branches into 5% solid content by using 0.075mol/L mixed aqueous solution of phosphotungstic acid and silicomolybdic acid, and soaking for 80 hours to ensure that the phosphotungstic acid and the silicomolybdic acid are fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating at 165 ℃ for 10 minutes to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing the grape branch fibers pretreated by heteropoly acid;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); after cooking, solid-liquid separation, washing with clear water to neutrality and drying are carried out to obtain grape branchesChemical pulp.
The grape branch chemical pulp obtained in the example has the yield of 29.53%, the content of alpha-cellulose of 94.04% and the alkali solubility S 10 And S 18 5.15% and 3.28%, respectively, and a kappa number of 4.58.
Example 7
(1) Pruning grape branches with the content of the holocellulose of 42.06% to be 2-3cm long, peeling off the skins of the grape branches, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the treated grape branches into 10% solid content by using 0.1mol/L aqueous solution of phosphotungstic acid, silicomolybdic acid and silicotungstic acid, and soaking for 120h to ensure that the phosphotungstic acid, silicomolybdic acid and silicotungstic acid are fully contacted with the grape branches;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution for 2 minutes at 180 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing grape branch fibers pretreated by heteropoly acid;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (the steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
(5) And (4) carrying out solid-liquid separation on the mixture in the step (3), and extracting and drying a liquid-phase product by using diethyl ether to obtain the recycled heteropoly acid.
The grape branch chemical pulp obtained in the example has the yield of 29.05 percent, the content of alpha-cellulose of 94.11 percent and the alkali solubility S 10 And S 18 4.93% and 3.22%, respectively, and a kappa number of 4.40; the recovery of heteropolyacid was 97.84%.
Example 8
(1) Pruning grape branches with the content of the holocellulose of 42.06% to be 2-3cm long, peeling off the skins of the grape branches, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the treated grape branches into 10% solid content by using 0.1mol/L aqueous solution of phosphotungstic acid, silicomolybdic acid and silicotungstic acid, and soaking for 120h to ensure that the phosphotungstic acid, silicomolybdic acid and silicotungstic acid are fully contacted with the grape branches; the mixture of phosphotungstic acid, silicomolybdic acid and silicotungstic acid used in this example was recovered as in example 7;
(3) placing the prepared grape branch/heteropoly acid solution in a high-temperature reaction kettle, and treating the grape branch/heteropoly acid solution for 2 minutes at 180 ℃ to ensure that the grape branch/heteropoly acid solution fully reacts to obtain a mixture containing grape branch fibers pretreated by heteropoly acid;
(4) separating solid from liquid, washing with clear water to neutrality, and steaming with sulfate (steaming condition is effective alkali: 16% (Na) 2 O meter), degree of vulcanization: 18% (Na) 2 Calculated as O), the solid-liquid ratio is 1:4, the cooking temperature is 140 ℃, and the heat preservation time is 40 min); and after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain the grape branch chemical pulp.
The grape branch chemical pulp obtained in the example has the yield of 29.14 percent, the content of alpha-cellulose of 93.94 percent and the alkali solubility S 10 And S 18 5.01% and 3.35%, respectively, and a kappa number of 4.54.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or equivalence to the invention are intended to be embraced therein.

Claims (4)

1. A prehydrolysis method for improving delignification efficiency of grape branches by a sulfate process is characterized by comprising the following steps of:
(1) pruning grape branches, peeling off the skins of the grape branches, sealing and storing at room temperature, and balancing water for later use;
(2) preparing the grape branches treated in the step (1) into a mixed solution with the solid content of 0.1-10% by using a heteropoly acid aqueous solution, and soaking to ensure that the heteropoly acid is fully contacted with the grape branches to obtain a grape branch/heteropoly acid suspension;
(3) treating the grape branch/heteropoly acid suspension prepared in the step (2) at 110-180 ℃ for 2-60 minutes to fully react to obtain a mixture containing grape branch fibers and heteropoly acid solution;
(4) carrying out solid-liquid separation on the mixture obtained in the step (3), washing the mixture to be neutral by using clear water, and then cooking the mixture by using a sulfate method; after cooking, carrying out solid-liquid separation, washing with clear water to neutrality, and drying to finally obtain grape branch chemical pulp;
pruning grape branches to be 2-3cm long in step (1);
in the step (1), the holocellulose content in grape branches is 40-80%, and the balance is the Clarsen lignin and ash;
in the step (2), the heteropoly acid is one or a mixture of more of phosphotungstic acid, silicotungstic acid and silicomolybdic acid;
the concentration of the heteropoly acid aqueous solution in the step (2) is 0.001-0.1 mol/L.
2. The prehydrolysis process for improving the delignification efficiency of the grape branch kraft process according to claim 1, characterized in that the soaking time in step (2) is 0.2-120 h.
3. The prehydrolysis method for improving delignification efficiency of grape branches by a sulfate process according to claim 1, characterized in that in the step (4), cooking conditions are effective alkali: 16% by weight of Na 2 O meter, degree of vulcanization: 18% by weight of Na 2 And (3) measuring the ratio of O to solid to liquid, wherein the cooking temperature is 140 ℃, and the heat preservation time is 40 min.
4. The prehydrolysis method for improving delignification efficiency of grape branches by the sulfate process according to claim 1, characterized in that, after the mixture is subjected to solid-liquid separation in step (4), the heteropoly acid in the liquid phase is recovered by ether extraction.
CN202110791842.3A 2021-07-13 2021-07-13 Prehydrolysis method for improving delignification efficiency of grape branches by sulfate process Active CN113564956B (en)

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