CN109706769B - Method for separating lignocellulose by blending small molecular aldehyde organic matter with organic acid - Google Patents
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Abstract
The invention relates to a method for separating lignocellulose by small molecular aldehyde organic matter blended organic acid, which mixes small molecular aldehyde organic matter and organic acid blend with a wood fiber raw material and then carries out high-temperature cooking. The process of the present invention is used for the separation of components of wood and non-wood fibre raw materials.
Description
Technical Field
The invention relates to a method for separating lignocellulose by blending small molecular aldehyde organic matters with organic acid, belonging to the field of biomass refining.
Background
The biomass raw material mainly comprises three major components of cellulose, hemicellulose and lignin, is the most abundant renewable resource on the earth, the total amount of lignocellulose resources generated by photosynthesis per year exceeds 2000 hundred million tons, and the biomass raw material is considered to be the best substitute for the traditional fossil raw material resources, however, in the existing traditional pulping and papermaking industry, only the cellulose in the plant fiber raw material is utilized, and a large amount of lignin is burnt in the alkali recovery process. This not only results in a significant waste of biomass resources, but also produces a considerable amount of CO2. In combination with the current problems of resource shortage, energy crisis, climate warming and the like in the global scope, the transformation and upgrading of the traditional pulping and papermaking industry are imminent. At present, the biomass refining mode combined with the pulping and papermaking industry is widely concerned by countries all over the world, wherein the construction of a biomass refining platform based on the technology of separating lignocellulose by an organic acid method can be provided withThe main components in the plant fiber raw material are effectively separated, the aim of efficiently separating the lignocellulose biomass is fulfilled by selectively dissolving lignin and hemicellulose, relatively pure cellulose pulp, lignin and hemicellulose saccharides are obtained, and the obtained organic acid lignin has the characteristics of no sulfur, high purity, good uniformity and high chemical reaction activity, and has higher utilization value and high-valued conversion potential. Therefore, the organic acid method separation technology is developed based on comprehensive, effective and high-value utilization of the wood fiber biomass, and the method has great significance for comprehensive utilization of resources and natural ecological environment.
The organic acid separation technology mainly uses formic acid, acetic acid or a mixed solution of the formic acid and the acetic acid as a cooking liquid medicine, and can also use a mixture of the organic acid and other organic solvents or inorganic catalysts for cooking.
For example, chinese patent ZL99805811.4 discloses a process for producing pulp using a mixture of formic acid and acetic acid as cooking chemicals. The method comprises the following steps: (1) a mixture of formic acid and acetic acid is used as a cooking medicine, wherein the formic acid content is 80-40%, the acetic acid content is 10-30%, the cooking temperature is 110-; (2) evaporating the used cooking liquor to solid content of 50-80%, and distilling to obtain mixture of formic acid and acetic acid for cooking.
Chinese patent document CN103924470A discloses a method for producing unbleached pulp with improved pulp whiteness. The method comprises the steps of pretreating the plant fiber raw material with sodium percarbonate, cooking by using a mixed organic solvent of formic acid, acetic acid and acetone, washing the cooked paper pulp with formic acid and hot water, and preparing the natural color paper pulp.
Chinese patent document zl02813978.x discloses a method for preparing pulp by cooking furfural-containing organic acids including formic acid and acetic acid. The method mainly comprises the following steps: (1) the mixture containing organic acid such as formic acid, acetic acid and the mixture thereof and furfural is used as a cooking reagent to be cooked at 105-160 ℃; (2) recovery of the cooking reagent comprising furfural obtained from the recovery step. Finally obtaining the pulp.
The traditional technology for preparing paper pulp by using organic acid cooking as organic acid has poor effect of removing lignin in raw materials, and a considerable amount of lignin is remained in the paper pulp, so that the consumption of subsequent bleaching reagents is increased; more importantly, as the organic acid dissolves out the lignin and the hemicellulose simultaneously in the cooking process, the subsequent recycling of dissolved-out lignin and hemicellulose resources is not involved, the waste of biomass resources is caused, and meanwhile, the adverse effect on the ecological environment is generated.
In order to improve the removal rate of lignin in the process of separating lignocellulose by organic acid, hydrogen peroxide, inorganic acid and other small molecular compounds are used as catalysts and added into a separation system for catalytic cooking.
Chinese patent document CN103898786A discloses a method for comprehensive utilization of biomass raw materials. The method mainly comprises the following steps: (1) under the catalytic action of hydrogen peroxide, utilizing organic acid liquor (total acid concentration is 70-85%) formed from formic acid and acetic acid to make digestion of pulverized biomass, controlling digestion temperature at 90-120 deg.C, solid-liquid mass ratio at 1:5-1:15, reaction time for 30-90min, and making solid-liquid separation after the reaction is completed; (2) pickling residual solids in a mixed solution formed by hydrogen peroxide, formic acid and acetic acid, then washing with water, and screening the obtained solids to obtain fine pulp cellulose; (3) and (3) evaporating and concentrating the digestion waste liquid and the pickling waste liquid to obtain formic acid, acetic acid steam and a concentrated solution, diluting the concentrated solution with water, stirring, washing the obtained solid with water to obtain the required lignin, and decoloring, filtering, concentrating and crystallizing the obtained liquid to obtain xylose.
Chinese patent document CN103122594A discloses a method for producing dissolving pulp. The method mainly comprises the following steps: (1) pre-hydrolyzing the fiber raw material by water, steam or dilute acid; (2) peroxide acid consisting of hydrogen peroxide and formic acid or acetic acid is used for cooking, and the cooking waste liquid is recycled after being distilled; (3) performing hemicellulase treatment on the slurry; (4) and (4) bleaching the pulp. Finally obtaining the dissolving pulp with the whiteness of more than 90 percent IS0, the alpha-cellulose content of more than 92 percent and the pentosan content of less than 2.0 percent.
The consumption of hydrogen peroxide in the organic acid cooking process using hydrogen peroxide as a catalyst is high, and the hydrogen peroxide is easily decomposed in a high-temperature environment to lose the catalytic performance. This process is only suitable for milder conditions, and the expected effect is achieved by increasing the number of reaction stages and increasing the reaction time, which undoubtedly increases the investment in equipment and the operating costs. The sulfuric acid is added in the process of separating the biomass by the organic acid method, so that the reaction strength of a separation system is increased, the partial degradation of cellulose is caused, the yield of paper pulp is reduced, the strength of the paper pulp is also obviously reduced, and the sulfur in the subsequently obtained lignin is inevitably contained.
In summary, in the existing research on biomass separation by an organic acid method, the removal efficiency of lignin is low, and in the process of organic acid separation of the lignocellulose biomass, a condensation reaction occurs while the lignin structure is depolymerized, so that the molecular weight of lignin is increased, and a very stable connecting bond is formed between lignin structural units, thereby not only reducing the lignin removal efficiency, but also increasing the difficulty in subsequent lignin depolymerization and reuse.
Therefore, a new technology for separating lignocellulose by organic acid is developed, so that the lignin removal rate is improved, and at the same time, no serious condensation reaction occurs, paper pulp with excellent performance and a micromolecule lignin product with higher yield are obtained, and the method has important significance for realizing high-valued and industrialized utilization of biomass resources.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for separating lignocellulose by blending small molecular aldehyde organic matters with organic acid.
Summary of the invention:
the invention utilizes the mixing of micromolecular aldehyde organic matters and organic acid to separate lignocellulose components, improves the lignin removal rate, inhibits the condensation reaction in the lignin removal process, obtains the lignin micromolecular product, and improves the economic feasibility of converting the lignin into high value-added compounds. Meanwhile, the residual lignin in the paper pulp is reduced, the bleaching energy consumption is reduced, and the quality of the pulp is improved. The operation flow is simple, the cooking time is short, and therefore, the production energy consumption and the operation cost are effectively reduced.
Detailed description of the invention:
the invention is realized by the following technical scheme:
a method for separating lignocellulose by blending small molecular aldehyde organic matters with organic acid comprises the following steps:
mixing the small molecular aldehyde organic matter and organic acid blend with wood fiber raw material;
the mixture is steamed at high temperature;
and separating paper pulp and lignocellulose after cooking.
According to the invention, the mixing step of the small molecular aldehyde organic matter and organic acid blend and the wood fiber raw material is as follows: mixing the micromolecular aldehyde organic matter and the organic acid according to the proportion to obtain a blend, and adding the wood fiber raw material into the blend to form a cooking system.
According to the invention, the volume ratio of the organic acid to the organic matter of the small-molecule aldehyde is (50-95): (5-50).
According to the invention, the organic acid is one or the combination of more than two of formic acid, acetic acid, oxalic acid or benzoic acid, and the mass concentration of the organic acid is 50-95%.
According to the invention, the small molecular aldehyde organic substance is one or the combination of two of formaldehyde, acetaldehyde, propionaldehyde and glyoxal.
According to the invention, the blend is prepared by mixing formic acid and formaldehyde or acetaldehyde according to the volume ratio of (60-90): (10-40) in the ratio of the total amount of the components.
Preferably, according to the invention, the mass-to-volume ratio of the amount of lignocellulosic feedstock added to the blend is: 1:4-1:20, unit: g/mL.
Preferably, according to the invention, the lignocellulosic feedstock comprises wood and non-lignocellulosic feedstock.
According to the invention, the mixture high-temperature cooking step is preferably as follows: the blend and the wood fiber raw material are combined into a cooking system to be cooked for 10-300min at the temperature of 60-170 ℃.
Preferably, the step of separating pulp and lignocellulose after cooking comprises: carrying out solid-liquid separation on the reactant after cooking to obtain solid and cooking waste liquid; the solid is washed by acid and water, pulp is obtained after screening, and the separated cooking waste liquid and the waste liquid after washing by acid are mixed to form black liquid; the black liquor is subjected to precipitation, evaporation, distillation and drying processes to recover organic acid, micromolecular aldehydes, lignocellulose and hemicellulose sugar from the black liquor.
The method of the present invention can be selected within a range of the kind, concentration and blending ratio of the organic acid and the small molecular aldehyde organic substance according to the structural characteristics of the lignocellulosic raw material and the delignification reaction kinetics thereof in an acidic environment, such as hardwood wood, softwood wood or non-wood lignocellulose.
The method for separating the lignocellulose component by using the micromolecular aldehyde organic matter blended with the organic acid is applied to the field of biomass refining.
Compared with the prior organic acid separation technology, the method has the following advantages
1. The method for separating lignocellulose by blending the micromolecular aldehyde organic matter with the organic acid has simple operation flow, does not introduce other inorganic acid and metal ions, and obtains purer products.
2. According to the method for separating lignocellulose by blending the micromolecular aldehyde organic matter with the organic acid, the micromolecular aldehyde organic matter is easy to recycle, and the production cost is reduced.
4. The method for separating lignocellulose by blending the micromolecular aldehyde organic matter with the organic acid improves the removal rate of lignin in the raw materials, the yield of the lignin is up to 35 percent, and the dosage of chemicals is reduced.
5. The method provided by the invention can inhibit lignin condensation reaction in the delignification process, is easy to obtain micromolecule lignin products, has high micromolecule lignin occupation ratio, and is beneficial to comprehensive and effective high-value utilization of lignocellulose biomass in the follow-up process.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following specific examples.
Examples 1,
A method for separating lignocellulose by blending acetaldehyde and formic acid comprises the following steps:
1) mixing acetaldehyde with formic acid with the mass concentration of 90% to obtain a blend, adding Ci bamboo chips into the blend to form a cooking system, wherein the length and width of the Ci bamboo chips are 2.0-4.0 cm, the thickness of the Ci bamboo chips is 0.5-1.0 cm, and the mass-volume ratio of the Ci bamboo chips to the blend is as follows: 1:10, unit: g/mL; the volume ratio of formic acid to acetaldehyde is: 6: 1;
2) the cooking system is put into a kettle and heated to 130 ℃, and the heating rate is 2.0 ℃/min. The cooking process is carried out in a Hastelloy C reaction kettle, and a heating sleeve with program temperature control is adopted for heating; cooking for 45 min;
3) filtering and washing: after cooking, solid-liquid separation is carried out to obtain black liquor and solid matters. And washing the solid matter with formic acid and hot water, and screening the pulp to obtain the paper pulp.
Chemical products such as formic acid, acetaldehyde, saccharides and lignin are recovered from the black liquor, and the organic acid and the acetaldehyde are recycled. Detection and analysis of the separated product: the yield of the pulp was 43%, the kappa number 17 and the viscosity 990.5 mg/L. The yield of lignin is 35.5%, wherein the content of small molecular lignin is 30%, and the weight average molecular weight and the number average molecular weight of lignin are 889g/mol and 795g/mol respectively.
Comparative examples 1,
A method for separating lignocellulose by using formic acid as cooking liquor, which is the same as the method in the example 1, and is characterized in that the cooking system only contains 90% of formic acid by mass concentration.
Detection and analysis of the separated product: the yield of the pulp was 40%, the kappa number was 35.5 and the viscosity was 1008.5 mg/L. The yield of lignin is 23.5%, the proportion of small molecular lignin is 3%, the weight average molecular weight and the number average molecular weight of lignin are 2891g/mol and 2153g/mol respectively, and in comparative example 1, only formic acid is used as cooking liquor, so that the lignin is easy to perform condensation reaction in the delignification process, and the proportion of small molecular lignin is smaller.
Examples 2,
A method for separating lignocellulose by mixing acetaldehyde with formic acid and acetic acid comprises the following steps:
1) mixing acetaldehyde with formic acid with the mass concentration of 90% and acetic acid with the mass concentration of 90% to obtain a blend, adding arrowroot bamboo chips into the blend to form a cooking system, wherein the length and width of the arrowroot bamboo chips are 2.0-4.0 cm, the thickness of the arrowroot bamboo chips is 0.5-1.0 cm, and the mass-volume ratio of the arrowroot bamboo chips to the blend is as follows: 1:10, unit: g/mL; the volume ratio of formic acid to acetic acid is 1: 1; the ratio of the total volume of formic acid and acetic acid to the volume of acetaldehyde is: 7: 3;
2) the cooking system is put into a kettle and heated to 130 ℃, and the heating rate is 2.0 ℃/min. The cooking process is carried out in a Hastelloy C reaction kettle, and a heating sleeve with program temperature control is adopted for heating; cooking for 45 min;
3) filtering and washing: after cooking, solid-liquid separation is carried out to obtain black liquor and solid matters. And washing the solid matter with formic acid and hot water, and screening the pulp to obtain the paper pulp.
Detection and analysis of the separated product: the yield of the pulp was 41.5%, the kappa number was 22.5 and the viscosity was 848.5 mg/L. The yield of the lignin is 30.5 percent, the ratio of the small molecular weight lignin is 28 percent, and the weight average molecular weight and the number average molecular weight of the lignin are 994g/mol and 853g/mol respectively.
Examples 3,
A method for separating lignocellulose by blending formaldehyde and formic acid comprises the following steps:
1) mixing formaldehyde and formic acid with the mass concentration of 90% to obtain a blend, adding Cizhu bamboo chips into the blend to form a cooking system, wherein the length and width of the Cizhu bamboo chips are 2.0-4.0 cm, the thickness of the Cizhu bamboo chips is 0.5-1.0 cm, and the mass-volume ratio of the Cizhu bamboo chips to the blend is as follows: 1:15, unit: g/mL; the volume ratio of formic acid to acetaldehyde is: 9: 4;
2) the cooking system is put into a kettle and heated to 100 ℃, and the heating rate is 2.0 ℃/min. The cooking process is carried out in a Hastelloy C reaction kettle, and a heating sleeve with program temperature control is adopted for heating; steaming for 180 min;
3) filtering and washing: after cooking, solid-liquid separation is carried out to obtain black liquor and solid matters. And washing the solid matter with formic acid and hot water, and screening the pulp to obtain the paper pulp.
Detection and analysis of the separated product: the yield of the pulp was 45.2%, the kappa number was 29.5 and the viscosity was 1022.5 mg/L. The yield of the lignin is 31.5 percent, the ratio of the small molecular weight lignin is 18 percent, and the weight average molecular weight and the number average molecular weight of the lignin are 669g/mol and 531g/mol respectively.
Examples 4,
A method for separating lignocellulose by blending formaldehyde and formic acid, which is the same as example 3, except that poplar wood chips are used for replacing Sasa sagittifolia bamboo chips, and the cooking temperature is 120 ℃.
Detection and analysis of the separated product: the yield of the pulp was 42.13%, the kappa number was 11.2 and the viscosity was 876.5 mg/L. The yield of the lignin is 29.2 percent, the proportion of the small molecular weight lignin is 37 percent, and the weight average molecular weight and the number average molecular weight of the lignin are 757g/mol and 698g/mol respectively.
Comparative examples 2,
A method for separating lignocellulose, which is the same as the embodiment 3, and is different in that macromolecular aldehyde organic matter benzaldehyde replaces formaldehyde to be mixed and separated at high temperature and high pressure, a cooking system is formic acid and benzaldehyde, and the rest is the same as the embodiment 3;
detection and analysis of the separated product: the yield of the pulp was 42.5%, the kappa number was 20.5 and the viscosity was 1008.5 mg/L. The yield of the lignin is 28.5 percent, the proportion of the small molecular weight lignin is 7 percent, and the weight average molecular weight and the number average molecular weight of the lignin are 852g/mol and 783g/mol respectively. Comparative example 2 adopts macromolecule aldehyde organic substance benzaldehyde and formic acid to form a cooking system, and the content of the obtained micromolecule lignin is also little.
Claims (2)
1. A method for separating lignocellulose by blending acetaldehyde and formic acid comprises the following steps:
1) mixing acetaldehyde with formic acid with the mass concentration of 90% to obtain a blend, adding Ci bamboo chips into the blend to form a cooking system, wherein the length and width of the Ci bamboo chips are 2.0-4.0 cm, the thickness of the Ci bamboo chips is 0.5-1.0 cm, and the mass-volume ratio of the Ci bamboo chips to the blend is as follows: 1:10, unit: g/mL; the volume ratio of formic acid to acetaldehyde is: 6: 1;
2) putting the cooking system into a kettle, heating to 130 ℃, and raising the temperature at the rate of 2.0 ℃/min;
the cooking process is carried out in a Hastelloy C reaction kettle, and a heating sleeve with program temperature control is adopted for heating; cooking for 45 min;
3) filtering and washing: after cooking, carrying out solid-liquid separation to obtain black liquor and solid matters;
washing the solid matter with formic acid and hot water, and screening the pulp to obtain paper pulp;
recovering formic acid, acetaldehyde, saccharides and lignin chemical products from the black liquor, and recycling the organic acid and the acetaldehyde;
detection and analysis of the separated product: the yield of the paper pulp is 43 percent, the kappa number is 17, and the viscosity is 990.5 mg/L;
the yield of lignin is 35.5%, wherein the content of small molecular lignin is 30%, and the weight average molecular weight and the number average molecular weight of lignin are 889g/mol and 795g/mol respectively.
2. A method for separating lignocellulose by mixing acetaldehyde with formic acid and acetic acid comprises the following steps:
1) mixing acetaldehyde with formic acid with the mass concentration of 90% and acetic acid with the mass concentration of 90% to obtain a blend, adding arrowroot bamboo chips into the blend to form a cooking system, wherein the length and width of the arrowroot bamboo chips are 2.0-4.0 cm, the thickness of the arrowroot bamboo chips is 0.5-1.0 cm, and the mass-volume ratio of the arrowroot bamboo chips to the blend is as follows: 1:10, unit: g/mL; the volume ratio of formic acid to acetic acid is 1: 1; the ratio of the total volume of formic acid and acetic acid to the volume of acetaldehyde is: 7: 3;
2) putting the cooking system into a kettle, heating to 130 ℃, and raising the temperature at the rate of 2.0 ℃/min;
the cooking process is carried out in a Hastelloy C reaction kettle, and a heating sleeve with program temperature control is adopted for heating; cooking for 45 min;
3) filtering and washing: after cooking, carrying out solid-liquid separation to obtain black liquor and solid matters;
washing the solid matter with formic acid and hot water, and screening the pulp to obtain paper pulp;
detection and analysis of the separated product: the yield of the paper pulp is 41.5 percent, the kappa number is 22.5, and the viscosity is 848.5 mg/L;
the yield of the lignin is 30.5 percent, the ratio of the small molecular weight lignin is 28 percent, and the weight average molecular weight and the number average molecular weight of the lignin are 994g/mol and 853g/mol respectively.
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| JP7242483B2 (en) * | 2019-09-12 | 2023-03-20 | 日華化学株式会社 | Cooking accelerator for lignocellulosic material and method for producing pulp using the same |
| EP3808755A1 (en) * | 2019-10-14 | 2021-04-21 | Ecole Polytechnique Federale De Lausanne (EPFL) EPFL-TTO | Production of fragments of lignin with functional groups |
| CN111979819B (en) * | 2020-08-10 | 2022-08-09 | 齐鲁工业大学 | Method for separating lignocellulosic biomass components |
| CN111958730B (en) * | 2020-08-10 | 2021-12-07 | 齐鲁工业大学 | Method for inhibiting lignin condensation |
| CN113445344A (en) * | 2021-07-29 | 2021-09-28 | 陕西科技大学 | Biomass refining method for removing lignin |
| CN114753177A (en) * | 2022-03-22 | 2022-07-15 | 齐鲁工业大学 | Method for separating biomass components by ternary system |
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