A production process of plant-derived fulvic acid based on taurine

Abstract

The present invention discloses a product and a production process for producing a plant-derived fulvic acid product with a high solid base content using taurine, belonging to the fields of biochemical engineering, fermentation engineering, biorefining, and synthetic biology industries. In the production process of the plant-derived fulvic acid product of the present invention, the raw materials are cooked and separated by the ammonium sulfite method to obtain fibers and fulvic acid. After adding a medicament containing taurine, it is mixed with liquid ammonium sulfite or solid ammonium sulfite dissolved in water and used as the cooking liquid medicine; after mixing the raw materials with the cooking liquid medicine, they are cooked, extracted, separated, and concentrated to obtain a concentrated dark liquid of fulvic acid with a high solid base content. The method of the present invention can increase the solid base content or dry base content of the plant-derived fulvic acid product. The detected value of the solid base content of the existing similar products of fulvic acid on the market is generally between 47% and 57%. According to the technical solution provided by the present invention for the plant-derived fulvic acid product, the increase range of the solid base content reaches 40% - 60%.

Description

Technical Field

[0001] The present invention belongs to the fields of biochemistry, comprehensive utilization of straw resources, separation of three elements, synthetic biological fermentation engineering and biomass energy, and relates to a plant-derived fulvic acid product and a preparation method thereof. Background Art

[0002] Taurine itself is a plant growth regulator, which has the effects of increasing crop growth, increasing yield, inhibiting the natural aging of crops, prolonging the lifespan of crops, improving stress resistance, and enhancing the rooting ability of crops. However, there is no report on the use of taurine for the preparation of fulvic acid.

[0003] Fulvic acid is considered a plant growth activator and is one of the humic acids with a relatively small molecular weight. Humic acid-based organic matter materials include water-soluble humic acid materials and water-insoluble humic acid materials. Water-soluble humic acid materials include water-soluble plant-derived sulfonated fulvic acid, water-soluble plant-derived biochemical fulvic acid, and water-soluble mineral-derived fulvic acid: Plant-derived sulfonated fulvic acid is a small molecular weight humic acid soluble in water obtained by sulfonation treatment of agricultural and forestry fruit waste including straw; Plant-derived biochemical fulvic acid is a water-soluble fulvic acid obtained by composting and fermenting straw with biological agents; Mineral-derived fulvic acid refers to a small molecular weight water-soluble humic acid soluble in water obtained by activating and extracting peat soil, lignite, and weathered coal by physical, chemical, and biological methods, with an average molecular weight of 50-100.

[0004] Currently, the preparation methods of fulvic acid mainly fall into four categories. The extraction method includes acid extraction, alkali extraction, acid-organic solvent extraction, and ion exchange resin method. The most important method for obtaining fulvic acid from weathered coal, lignite, peat, etc. is the extraction method. The fermentation method uses mainly some industrial and agricultural waste materials, sawdust, etc. as raw materials, adds appropriate amounts of nutrients such as nitrogen, phosphorus, and potassium, first reacts using biological fermentation technology to obtain a fermentation material rich in fulvic acid, and then extracts a product rich in fulvic acid from the fermentation material through leaching. The electrodialysis method belongs to a method of deep purification and is generally used for further processing and purification of fulvic acid crude products. The extraction method is to use ammonium bisulfite as an auxiliary agent to obtain a plant-derived fulvic acid product and cellulose pulp through cooking and extraction.

[0005] The patent with the publication number CN 208308727 U discloses a preparation system for a fulvic acid potassium phosphite ammonium phosphate solid compound fertilizer. By granulation, a potassium phosphite solution, an ammonium phosphate solution, and a potassium fulvate solution are mixed to generate a fulvic acid potassium phosphite ammonium phosphate solid compound fertilizer.

[0006] The patent application with the publication number CN 102328963 A discloses the preparation of a black crystal aquaculture synergist containing fulvic acid using weathered coal and sodium hydroxide as raw materials: weathered coal is extracted with a sodium hydroxide solution under heating conditions, and after filtration, a soy sauce-colored solution containing free humic acid is obtained. Then, the soy sauce-colored solution is acidified with a hydrochloric acid solution, and after filtration, a fulvic acid solution is obtained. Next, sodium hydroxide is added to the fulvic acid solution and reacted under heating conditions, and the resulting solid is dried, crushed, and sieved to obtain the black crystal aquaculture synergist.

[0007] The patent with the publication number CN 114044717 A includes the following steps: 1) Crushing and dissolving inorganic raw materials: The proportioned solid raw materials including urea, monoammonium phosphate, potassium tripolyphosphate, diammonium phosphate, and boric acid are crushed by a raw material crushing device and placed in a reaction kettle, and proportioned soft water is added for dissolution; 2) Dissolving auxiliary materials: Fish protein powder, seaweed essence, potassium fulvate, NAM inhibitor, and phosphorus element activator are added to the reaction kettle for dissolution; 3) Mixing and stirring; 4) Subcontracting; 5) Packaging to obtain a special liquid fertilizer for cotton.

[0008] The invention with the publication number CN105503475A discloses a microencapsulated amino acid liquid mineral fertilizer, which uses an aqueous sodium hydroxide solution as a raw material and is prepared into a finished product through the production and microencapsulation of liquid fertilizers and solid fertilizers.

[0009] However, the key problem of using plant-derived fulvic acid products as renewable biochemistry raw materials is how to high-quality separate its solid base content (mainly composed of cellulose, hemicellulose, and lignin) to obtain raw materials for large-scale utilization for downstream conversion. In the past, through chemical treatment methods such as acids, alkalis, and organic solvents, partial separation of lignin, hemicellulose, and cellulose components could be achieved, but usually only one or two components (mainly cellulose components) could be utilized, and it was difficult to achieve high-value utilization of the three components. Therefore, how to increase the solid base content of plant-derived fulvic acid products and enhance their application value is an important topic in this field. Summary of the Invention

[0010] The technical problem to be solved by the present invention is to increase the solid base content of fulvic acid, that is, the content of fulvic acid in the dry basis state, to break through the upper limit of the commonly used fulvic acid content at present, so as to improve the application efficiency and reduce the production cost.

[0011] The increase in the solid base content of fulvic acid can increase the efficacy of fulvic acid per unit weight or unit volume, improve the effective yield of fulvic acid, and reduce the production cost of fulvic acid from straw raw materials. The difficulty in the process lies in finding a suitable agent to achieve the effect of increasing the solid base content of fulvic acid produced by the ammonium sulfate method.

[0012] The fixed-base content of fulvic acid refers to the content of fulvic acid in the dry-base state. The fixed-base content of fulvic acid on the market is generally 40%-60%. Among them, the estimated content of mineral-source fulvic acid (potassium) is 55%; for plant-source fulvic acid products, the highest is 60%, and generally 43%; for molasses fulvic acid, the highest value is 60%.

[0013] To solve the technical bottlenecks in production practice, the present invention proposes a technical solution for producing plant-source fulvic acid with a high fixed-base content using sodium sulfite and taurine as the core.

[0014] In the first aspect, the present invention provides a product for producing a plant-source fulvic acid product with a high fixed-base content using taurine and its production process.

[0015] The plant-source fulvic acid product produced by the present invention using taurine has a pH of 5-6 for the concentrated fulvic acid stock solution obtained after concentration, and a solid content of not less than 55% by mass percentage. Preferably, the fixed-base content of the concentrated fulvic acid product reaches 60%-80%.

[0016] Correspondingly, the present invention provides a production process for producing a plant-source fulvic acid product with a high fixed-base content using taurine. The addition order of each raw material component is as follows: first, dissolve the medicament in water, and then synchronously load it into the cooking vessel with ammonium sulfite solid or liquid and the raw materials, and load the pot according to the set liquid ratio.

[0017] Specifically, the production process includes:

[0018] S1, obtaining raw materials;

[0019] S2, obtaining the medicament SYS;

[0020] S3, mixing the medicament SYS with liquid ammonium sulfite or solid ammonium sulfite dissolved in water to form a cooking liquid;

[0021] S4, mixing the raw material cooking liquid with the cooking liquid, and sequentially completing cooking extraction, separation, and concentration to obtain a concentrated dark fulvic acid liquid with a high fixed-base content;

[0022] The medicament SYS includes taurine and magnesium sulfate;

[0023] The addition amount of taurine is not less than 0.1% of the weight of the raw materials, and magnesium sulfate is 0.2%-2%.

[0024] The core medicament SYS (the core medicament is also called the medicament, medicament SYS, etc.) includes taurine and magnesium sulfate. The specific combinations include salicylic acid plus magnesium sulfate, taurine plus magnesium sulfate, or taurine plus salicylic acid plus magnesium sulfate, etc.

[0025] In the core medicament of the present invention, adding taurine can not only increase the solid base content of the plant-derived fulvic acid product, but also give full play to the role of taurine in agriculture.

[0026] In the production process of using taurine to produce a plant-derived fulvic acid product with a high solid base content described in the present invention, the neutral ammonium sulfite method is adopted for cooking, with a pH value of 6 - 9, to obtain fibers and raw material cooking liquor. The pH of the concentrated fulvic acid stock solution is 5 - 6, and the solid content is not less than 60% by mass percentage. The solid content refers to the content of solids, which is different from the solid base content. Here, the solid content refers to the mass percentage of the solid mass in the fulvic acid stock solution.

[0027] Preferably, the cooking temperature range is 160 - 180 °C, more preferably 160 - 175 °C, such as 165 °C, 168 °C, 170 °C, 173 °C, etc.

[0028] The heat preservation time range is 30 - 120 min. Preferably, the heat preservation time range is 50 - 100 min.

[0029] In the present invention, the addition amounts of the components in the core medicament SYS are in terms of the mass percentage of the dry raw material. The dosage of the medicament SYS is 1% - 10% of the weight of the raw material. Preferably, the dosage of the medicament SYS is 3% - 5% of the weight of the raw material by mass percentage. The plant-derived fulvic acid product produced retains the component of taurine. Among them, the addition amount of taurine is 0.1% - 10%, preferably 0.5% - 5%, 1% - 5% of the weight of the raw material, and more preferably 2% - 3%, such as 1.2%, 1.5%, 1.6%, 1.8%, 2%, 2.2%, 2.5%, 2.6%, 2.8% by mass percentage. In a preferred example of the present invention, the addition amount of taurine is 1%.

[0030] Preferably, ammonium sulfite is added in the preparation process of the present invention, and the dosage of ammonium sulfite is 15% - 35% of the weight of the raw material by mass percentage. More preferably, the dosage of ammonium sulfite is 18% - 35% of the weight of the dry raw material by mass percentage. The weight of the dry raw material refers to the weight of the raw material converted to the dry basis state.

[0031] Correspondingly, the present invention provides a product of using taurine to produce a plant-derived fulvic acid with a high solid base content. In this plant-derived fulvic acid product, the finished plant-derived fulvic acid produced by adopting this technical solution contains taurine.

[0032] In the second aspect, the present invention provides a medicament for the production process of using taurine to produce a plant-derived fulvic acid product with a high solid base content. The medicament contains taurine and magnesium sulfate; the content of taurine accounts for 0.1% - 10% of the weight of the raw material, and magnesium sulfate is 0.2% - 2% by mass percentage.

[0033] Preferably, the core agent in the present invention may also contain salicylic acid. The addition amount of salicylic acid is not less than 0.1% and not more than 3% of the raw material mass, excluding the end values. More preferably, it is not less than 0.5%, such as 0.5% - 2.0%. When salicylic acid is added to the core agent at this concentration, it can further promote the increase of the fulvic acid content in the product, especially the fulvic acid content in the solid product after drying.

[0034] In the third aspect, the present invention provides the application of the production process of using taurine to produce a plant-derived fulvic acid product with a high solid base content. When using the said production process to produce fulvic acid, the solid base content of the produced fulvic acid is not less than 57%.

[0035] Currently, the solid base content of most fulvic acid products on the market is less than 50%. The solid base content of the fulvic acid product of the present invention is not less than 57%, and even higher than 60%, by mass percentage. This can greatly improve the application value and use efficiency of the product. The tests of the present invention show that, compared with the fulvic acid with a relatively high solid base content on the current market (the solid base content of fulvic acid is less than 50%), using the fulvic acid with a high solid base content significantly enhances the root development of wheat, manifested as strong rhizomes and white and vigorous roots. When using a product with a fulvic acid solid base content greater than 70% to apply to wheat, the average root length of wheat after 20 days is nearly 3 times that of using the fulvic acid with a relatively high solid base content on the current market.

[0036] Preferably, neutral ammonium sulfite method is adopted for cooking, with pH 6 - 9, using a non - Na ion buffer, to obtain fibers and raw material cooking liquor; cooking at 160 - 173 °C for 30 - 120 min with heat preservation.

[0037] Preferably, the core agent SYS includes taurine, salicylic acid, magnesium sulfate, etc., all of which are commercially available.

[0038] Preferably, the temperature is raised and heat is preserved according to the ammonium sulfite pulping process. The cooking temperature and heat preservation time are set according to the different requirements of raw materials and target pulp properties.

[0039] Preferably, the dosage of the core additive SYS is 0.1% - 10% of the raw material weight, preferably 0.5% - 5%, by mass percentage.

[0040] The dosage of taurine in the core additive SYS is not less than 0.1% of the raw material weight, and more preferably not less than 1%. For example, the dosage of taurine is 0.5% - 10%, 1% - 8%, 3% - 5%, and 1 - 2% of the raw material, etc., by mass percentage.

[0041] In the present invention, the core auxiliary agent SYS also contains salicylic acid, and the content of salicylic acid is not more than 3%. Preferably, the content of salicylic acid is not more than 2%. In the core auxiliary agent SYS of the present invention, the addition amount of taurine can be 0.1-3% of the weight of the raw materials, magnesium sulfate can be 0.5%-2% of the weight of the raw materials, and the content of salicylic acid can be 0.1%-3% of the weight of the raw materials, by mass percentage. More preferably, the addition amount of taurine is 0.5-1% of the weight of the raw materials, magnesium sulfate is 0.5%-1% of the weight of the raw materials, and the content of salicylic acid is 0.5%-2% of the weight of the raw materials, by mass percentage.

[0042] In the present invention, the raw materials for producing fulvic acid are selected from various plants or their wastes: one or more of corn straw, corncob, lignin sludge, bamboo, reed, cotton straw, wheat straw, and rice straw. For example, in the plant-derived fulvic acid product obtained from the corncob raw material in Linyi, the content of fulvic acid is 75.79% and the content of water-soluble humic acid is 78.71%, by mass percentage. In another preferred example, using bamboo chips raw material from Jiangxi, 30% of ammonium sulfite, 5% of taurine, and 0.5% of magnesium sulfate, 71.3% of fulvic acid is obtained with a pH of 5.6. In yet another preferred example, using bamboo block raw material, 2% of salicylic acid, 30% of ammonium sulfite, 0.5% of magnesium sulfate, and 1% of taurine, 72.7% of fulvic acid is obtained.

[0043] Preferably, after adding the core auxiliary agent SYS, the component of taurine is retained in the plant-derived fulvic acid product produced. Preferably, the finished product of the plant-derived fulvic acid product produced by this technical solution contains fulvic acid, taurine, ammonium sulfate, ammonium sulfite, and salicylic acid. For the production process of adding salicylic acid to the core agent, a certain amount of salicylic acid component is retained in the finally obtained fulvic acid product.

[0044] The plant-derived fulvic acid product described in the present invention is a small-molecular-weight fulvic acid obtained by sulfonation treatment of non-wood fiber biomass fiber raw materials, and its indexes are: fulvic acid > 60%, preferably the content of fulvic acid is greater than 75%, the organic matter content is 50%-70%, the humic acid content is 60%-70%, the humic acid is 0.2%-0.36%, the average molecular weight < 50, the proportion of the molecular weight < 180 is > 95%, and the pH is 4-6.

[0045] In the present invention, the detection method for the SYS component in fulvic acid adopts NMR, MS, and HPLC. The detection standard for fulvic acid refers to HG / T 5332-2018 "Humic Acid Bio-organic Fertilizer".

[0046] In the method of the present invention, after adding the core auxiliary agent SYS, the solid base content of fulvic acid can be significantly increased. It is increased by 40%, for example, from 40%-50% to 70% or even higher.

[0047] Fourthly, the present invention provides a plant-derived fulvic acid product.

[0048] Using a core agent containing taurine to produce a plant-derived fulvic acid product with a high solid-based content, the pH of the concentrated fulvic acid stock solution is 5-6, and the solid content is not less than 55%-57% by mass percentage. Preferably, the solid-based content of the produced fulvic acid is not less than 60%.

[0049] The plant-derived fulvic acid product with a high solid-based content of the present invention can be used as a chemical fertilizer, soil conditioner, plant growth promoter, nutrient solution additive, etc. The plant raw materials used for producing fulvic acid include but are not limited to one or more of corn straw, corn cob, lignin sludge, bamboo, reed, cotton straw, wheat straw, and rice straw.

[0050] In the description of the present invention, the terms "comprising", "including" or any other variation thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements but also includes other elements not expressly listed, or further includes elements inherent to such process, method, article or device. Without further limitation, an element defined by the statement "comprising a reference structure" does not exclude the presence of additional identical elements in the process, method, article or device comprising the element. It should be noted that in this text, relational terms such as "first", "second", etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations.

[0051] The beneficial effects of the present invention include:

[0052] 1. Significantly improve the solid-based content of the plant-derived fulvic acid product, from 40%-50% to 60% or even more than 70%, and the improvement rate is at least over 40%. It far exceeds the common fulvic acid products on the market, including mineral-source fulvic acid, molasses fulvic acid, and similar plant-derived fulvic acid products.

[0053] 2. The increase in the solid-based content of fulvic acid improves the effective content of fulvic acid per unit weight or volume, reduces transportation costs, and improves the feasibility of fertilizer substitution, which can effectively promote fertilizer reduction and efficiency increase.

[0054] 3. Improve the production efficiency of the plant-derived fulvic acid product, with a high marginal return rate, greatly improve the production efficiency, and improve the carbon emission effect.

[0055] 4. The taurine contained in fulvic acid greatly enhances the comprehensive function of the plant source, forming a functional superposition of fulvic acid and taurine. Detailed implementation mode

[0056] The present invention provides a method for producing a plant-derived fulvic acid product with a high solid base content using salicylic acid and a production process. The raw materials and method for a complete production process of a plant-derived fulvic acid product with a high solid base content are as follows:

[0057] (1) Raw materials: Using Hegang corncob xylose residue as the raw material.

[0058] (2) Medicine preparation: Preparation of SYS liquid medicine. The core medicine is mainly in solid form, calculated by the mass of the raw materials; Dilute the medicine at a ratio of 1:10 - 30 and set aside;

[0059] Taking the dosage of solid ammonium sulfite as 30% as an example, calculated by the mass of the raw materials.

[0060] (3) Cooking method: Adopt intermittent spherical digester cooking.

[0061] (4) Loading the digester:

[0062] When using solid ammonium sulfite, the raw materials, ammonium sulfite, and SYS liquid medicine are added proportionally along with the conveyor belt for transportation.

[0063] When using liquid ammonium sulfite, first form a mixed solution of SYS liquid medicine and liquid ammonium sulfite, and then add the mixed solution and the raw materials proportionally for transportation.

[0064] If using liquid ammonium with a solid content of 30%, the water addition amount is (1 + 0.002 + 0.002 + 0.002 + 0.3) × 3.5 - 0.7 = 3.8 tons.

[0065] (5) Cooking. Heat up to 170 °C and keep warm for 70 min.

[0066] (6) Blow-off.

[0067] (7) Solid-liquid separation. Conduct solid-liquid separation in a conventional manner. In this scheme, a screw press is used to separate straw cellulose and fulvic acid black liquor, and four-stage reverse washing is adopted to obtain dilute fulvic acid black liquor and crude cellulose pulp.

[0068] (8) Concentration of fulvic acid black liquor. The dilute fulvic acid black liquor is concentrated through multi-effect evaporation to obtain concentrated fulvic acid black liquor.

[0069] (9) Drying. Spray-dry the concentrated fulvic acid black liquor to obtain fulvic acid dry powder.

[0070] (10) Test results.

[0071] The solid base content of fulvic acid refers to the content of fulvic acid in the dry base state. It is necessary to dry the fulvic acid product into dry powder and then detect the content of fulvic acid and calculate. The corresponding calculation formula:

[0072] Fixed base content = weight of fulvic acid (FA) / total weight of plant-derived fulvic acid product (dry basis) %, mass percentage.

[0073] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0074] Example 1

[0075] (1) Raw material: bamboo chips.

[0076] (2) Production process, same as the steps and methods of the above embodiment.

[0077] (3) Medicament formula: magnesium sulfate 0.5%, taurine 0.5%.

[0078] (4) Test result: fulvic acid (dry basis) 61.2%.

[0079] The above results show that by adding taurine to the core medicament and cooperating with magnesium sulfate, and using the ammonium sulfite method to produce with plant raw materials, the fixed base content of the obtained fulvic acid product is significantly improved.

[0080] Example 2

[0081] (1) Raw material: bamboo blocks.

[0082] (2) Production process, same as Example 1.

[0083] (3) Medicament formula: magnesium sulfate 0.2%, taurine 1%.

[0084] (4) Test result: fulvic acid (dry basis) 62.9%.

[0085] The above results show that the production process of the present invention can not only use bamboo chips as raw materials, but also use bamboo blocks as raw materials. Both bamboo chips and bamboo blocks can be taken from common bamboo forests and are usually used as wastes. By adding taurine to the core medicament in the present invention and using the ammonium sulfite method to produce the originally waste plant raw materials, the fixed base content of the obtained fulvic acid product is significantly improved, and it is also more environmentally friendly.

[0086] Example 3

[0087] (1) Raw material: lignin sludge.

[0088] (2) Production process, same as Example 1.

[0089] (3) Medicament formula: magnesium sulfate 15%, taurine 5%.

[0090] (4)Detection result: Fulvic acid (dry basis) 69.0%.

[0091] The above results indicate that the production process of the present invention is also applicable to the common lignin sludge in the soil.

[0092] Example 4

[0093] (1)Raw material: Xylose residue.

[0094] (2)Production process, the same as in Example 1.

[0095] (3)Reagent formula: Magnesium sulfate 0.5%, Taurine 2%.

[0096] (4)Detection result: Fulvic acid (dry basis) 67.5%.

[0097] The above results indicate that the production process of the present invention is also applicable to xylose residue.

[0098] Example 5

[0099] (1)Raw material: Reed.

[0100] (2)Production process, the same as in Example 1.

[0101] (3)Reagent formula: Magnesium sulfate 2%, Taurine 5%.

[0102] (4)Detection result: Fulvic acid (dry basis) 72.9%.

[0103] The above results indicate that the production process of the present invention is also applicable to reed.

[0104] Example 6

[0105] (1)Raw material: Corn straw.

[0106] (2)Production process, the same as in Example 1. Ammonium sulfite 20%.

[0107] (3)Reagent formula: Magnesium sulfate 0.5%, Taurine 0.1%.

[0108] (4)Detection result: Fulvic acid (dry basis) 41.8%.

[0109] The above results indicate that too low addition of taurine or reduction of the amount of ammonium sulfite will result in a low content of the obtained fulvic acid product in the dry basis state. Although it is also applicable and has a higher fulvic acid solid content than many similar products currently sold and used in the market, its effect still needs to be improved for applications such as high - requirement fertilizers or soil conditioners.

[0110] Example 7

[0111] (1)Raw materials: corn straw.

[0112] (2)Production process: same as Example 1, but with 20% ammonium sulfite.

[0113] (3)Agent formula: 0.5% magnesium sulfate, 0.5% taurine.

[0114] (4)Test results: fulvic acid (dry basis) 48.0%.

[0115] The above results show that under the same addition amounts of magnesium sulfate and ammonium sulfite and production process conditions, increasing the dosage of taurine helps to increase the solid-based content of fulvic acid. A proportion of 0.4% of the raw material content can significantly increase the content of fulvic acid. However, generally speaking, the combined action of the core agent and related components is required to further increase the absolute quantity of the solid-based content of fulvic acid.

[0116] Example 8

[0117] (1)Raw materials: corn straw.

[0118] (2)Production process: same as Example 1.

[0119] (3)Agent formula: 0.5% magnesium sulfate, 1.0% taurine.

[0120] (4)Test results: fulvic acid (dry basis) 64.0%.

[0121] The above results show that increasing the dosage of taurine helps to increase the solid-based content of fulvic acid. A proportion of 1.0% of the raw material content of taurine can significantly increase the content of fulvic acid - exceeding 60%. Compared with the fulvic acid products on the market with a relatively high content of 45% - 50%, the solid-based content of fulvic acid of the present invention has increased by more than 20%.

[0122] Example 9

[0123] (1)Raw materials: corn straw.

[0124] (2)Production process: same as Example 1.

[0125] (3)Agent formula: 0.5% magnesium sulfate, 3.0% taurine.

[0126] (4)Test results: fulvic acid (dry basis) 70.6%.

[0127] The above results show that, under the same addition amounts of magnesium sulfate and ammonium sulfite and production process conditions, increasing the dosage of taurine helps to increase the solid-based content of fulvic acid. A taurine proportion of 3.0% in the raw materials can make the content of fulvic acid exceed 70%. Compared with the fulvic acid products on the market with a relatively high content of 45%-50%, the solid-based content of the fulvic acid in the present invention has increased by more than 40%.

[0128] Example 10

[0129] (1) Raw materials: Corn straw.

[0130] (2) Production process, the same as in Example 1.

[0131] (3) Medicament formula: Magnesium sulfate 0.5%, taurine 5%.

[0132] (4) Test results: Fulvic acid (dry basis) 75.7%.

[0133] The above results show that increasing the dosage of taurine helps to increase the solid-based content of fulvic acid. A taurine proportion of 5.0% in the raw materials can make the content of fulvic acid exceed 75%. Compared with the fulvic acid products on the market with a relatively high content of 45%-50%, the solid-based content of the fulvic acid in the present invention has increased by 50% or more. However, compared with the case of a lower taurine content, after the taurine proportion in the raw materials reaches 5.0%, the increasing effect ratio of the further taurine content on the solid-based content of fulvic acid is not as obvious as before.

[0134] Example 11

[0135] (1) Raw materials: Corn straw.

[0136] (2) Production process, the same as in Example 1.

[0137] (3) Medicament formula: Magnesium sulfate 0.5%, salicylic acid 0.5%, taurine 0.1%.

[0138] (4) Test results: Fulvic acid (dry basis) 73.4%.

[0139] The above results show that in the presence of taurine, adding salicylic acid can increase the solid-based content of fulvic acid.

[0140] Example 12

[0141] (1) Raw materials: Corn straw.

[0142] (2) Production process, the same as in Example 1.

[0143] (3) Medicament formula: Magnesium sulfate 0.5%, salicylic acid 1.0%, taurine 0.5%.

[0144] (4)Test result: Fulvic acid (dry basis) 75.3%.

[0145] The above results show that in the presence of taurine, increasing salicylic acid can increase the solid basis content of fulvic acid. However, significantly increasing the content of taurine or salicylic acid does not further significantly increase the solid basis content of fulvic acid as expected.

[0146] Example 13

[0147] (1)Raw material: Corn straw.

[0148] (2)Production process: The same as that of Example 1.

[0149] (3)Agent formula: Magnesium sulfate 0.5%, salicylic acid 1%, taurine 1%.

[0150] (4)Test result: Fulvic acid (dry basis) 72.6%.

[0151] The above results show that in the presence of taurine, increasing salicylic acid can increase the solid basis content of fulvic acid. However, significantly increasing the content of taurine or salicylic acid does not further significantly increase the solid basis content of fulvic acid as expected. Moreover, in this example, the content of taurine is further increased, but the dry basis content of fulvic acid does not increase further.

[0152] Example 14

[0153] (1)Raw material: Corn straw.

[0154] (2)Production process: The same as that of Example 1.

[0155] (3)Agent formula: Magnesium sulfate 0.5%, salicylic acid 2%, taurine 0.5%.

[0156] (4)Test result: Fulvic acid (dry basis) 75.8%.

[0157] The above results show that in the presence of relatively high dosages of taurine and salicylic acid, further increasing salicylic acid does not further significantly increase the solid basis content of fulvic acid as expected.

[0158] Example 15

[0159] (1)Raw material: Corn straw.

[0160] (2)Production process: The same as that of Example 1.

[0161] (3)Agent formula: Magnesium sulfate 0.5%, salicylic acid 2%, taurine 1.0%.

[0162] (4)Test result: Fulvic acid (dry basis) 72.5%.

[0163] The above results show that in the presence of relatively high dosages of taurine and salicylic acid, increasing both salicylic acid and taurine simultaneously does not further significantly increase the fixed-base content of fulvic acid as expected. Instead, it may lead to a decrease in the content of fixed-base fulvic acid in the fulvic acid product.

[0164] Example 16

[0165] (1) Raw material: Corn straw.

[0166] (2) Production process: The same as that in Example 1.

[0167] (3) Medicament formula: Magnesium sulfate 0.5%, salicylic acid 3%, taurine 0.5%.

[0168] (4) Test result: Fulvic acid (dry basis) 73.3%.

[0169] Example 17

[0170] (1) Raw material: Corn straw.

[0171] (2) Production process: The same as that in Example 1.

[0172] (3) Medicament formula: Magnesium sulfate 1.0%, taurine 0.5%.

[0173] (4) Test result: Fulvic acid (dry basis) 72.0%.

[0174] The results of Examples 16 and 17 show that in the presence of relatively high dosages of taurine and salicylic acid, further increasing salicylic acid may instead lead to a slight decrease in the content of fixed-base fulvic acid in the fulvic acid product.

[0175] Control group

[0176] Compared with Example 1, fulvic acid is produced using corncob xylose residue as the raw material.

[0177] (1) Raw material: Taking Hegang corncob xylose residue as an example.

[0178] (2) Medicine preparation: Prepare the SYS liquid medicine according to the predetermined dosage. For example: acetic acid 2%, magnesium sulfate 0.5%, both are solids, calculated based on the mass of the raw material. Dilute the medicine with purified water in a volume ratio of 1:10 - 30 and set aside.

[0179] The dosage of solid ammonium sulfite (which can be simply referred to as ammonium) is 30%, calculated based on the mass of the raw material.

[0180] (3) Cooking method: Use intermittent spherical digester for cooking.

[0181] (4) Loading the digester:

[0182] When solid ammonium sulfite is used, the raw materials, ammonium sulfite, and SYS liquid medicine are added and conveyed proportionally along with the conveyor belt.

[0183] When liquid ammonium sulfite is used, first, the SYS liquid medicine and liquid ammonium sulfite are formed into a mixed liquid, and then the mixed liquid and the raw materials are added and conveyed according to a ratio.

[0184] If liquid ammonium sulfite with a solid content of 30% is used, the water addition amount is (1 + 0.002 + 0.002 + 0.002 + 0.3) × 3.5 - 0.7 = 3.8 tons.

[0185] (5) Cooking. Heat up to 170°C and keep warm for 70 min.

[0186] (6) Blowdown.

[0187] (7) Solid-liquid separation. Solid-liquid separation is carried out by a conventional method. In this scheme, a screw press is used to separate straw cellulose and fulvic acid black liquor, and four-stage countercurrent washing is adopted to obtain fulvic acid dilute black liquor with a solid content of 16% and cellulose coarse pulp.

[0188] (8) Concentration of fulvic acid black liquor. The 16% fulvic acid dilute black liquor is concentrated by multi-effect evaporation to obtain a commercial fulvic acid concentrated black liquor with a solid content of 55% (volume concentration).

[0189] (9) Drying. The fulvic acid concentrated black liquor with a solid content of 55% is spray-dried to obtain fulvic acid dry powder.

[0190] (10) Test results.

[0191] Test indicators: fulvic acid (dry basis) 51.08%, water-soluble humic acid content 54.65%, carboxyl group 0.26 (ad mmol / g), phenolic hydroxyl group 0.08 (ad mmmol / g).

[0192] The results of the comparative example show that although both acetic acid and taurine can be used in the production of fulvic acid products, and the obtained dry basis content of fulvic acid is also relatively high. However, after adding the same content of acetic acid, the obtained solid basis content of fulvic acid is 51.1%, while after adding taurine selected in the present invention, the obtained solid basis content of fulvic acid is 67.4%, and the improvement ratio reaches 32%. Whether this high-solid-basis fulvic acid product is used for fertilizers, improving soil texture, or other purposes, it has higher efficiency and lower cost than existing fulvic acid products.

[0193] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A production process of plant-derived fulvic acid based on taurine, characterized in that, The described production process includes: S1, obtaining raw materials; S2, obtaining the medicament SYS; S3, mixing the medicament SYS with ammonium sulfite to form a cooking liquor; S4, mixing the raw material cooking liquor with the cooking liquor, and then sequentially completing cooking, extraction, separation, and concentration to obtain a fulvic acid concentrated black liquor with a high solid content; The described medicament SYS includes taurine and magnesium sulfate; The dosage of taurine is 2% - 5% of the weight of the raw materials, and magnesium sulfate is 0.2% - 2% of the weight of the raw materials, by mass percentage.

2. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, The dosage of ammonium sulfite is 15% - 35% of the weight of the raw materials, by mass percentage.

3. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, The dosage of the medicament SYS is 3% - 10% of the weight of the raw materials, by mass percentage; Using plant raw materials to carry out cooking by the neutral ammonium method, with a pH value of 6 - 9, to obtain fibers and a raw material cooking liquor. After concentration, the pH of the obtained fulvic acid stock solution is 5 - 6, and the solid content is not less than 55%, by mass percentage; The cooking temperature range is 160 - 180°C, and the heat preservation time range is 30 - 120 min.

4. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, The dosage of taurine in the medicament SYS is 3% - 5% of the weight of the raw materials, by mass percentage.

5. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, The dosage of ammonium sulfite is 20% - 30% of the weight of the raw materials in the dry basis state, and the dosage of taurine in the medicament SYS is 2% - 3% of the weight of the raw materials, by mass percentage.

6. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, Magnesium sulfate is 0.5% - 2% of the weight of the raw materials, by mass percentage.

7. The production process of plant-derived fulvic acid based on taurine according to claim 1, characterized in that, The described medicament SYS also contains salicylic acid, and the content of salicylic acid is not more than 3%.

8. The production process of plant-derived fulvic acid based on taurine according to claim 7, characterized in that, The content of salicylic acid is not more than 2%.

9. The production process of plant-derived fulvic acid based on taurine according to claim 7, characterized in that, Magnesium sulfate is 0.5% - 2% of the weight of the raw materials, and the content of salicylic acid is 0.1% - 3% of the weight of the raw materials, by mass percentage.

10. The production process of plant-derived fulvic acid based on taurine according to claim 7, characterized in that, Magnesium sulfate is 0.5% - 1% of the weight of the raw materials, and the content of salicylic acid is 0.5% - 2% of the weight of the raw materials, by mass percentage.