High-solid-based plant-derived fulvic acid produced using hops and production process

By using hops and core additive SYS for imimide treatment, the solid-base content of chlorophyllium acid is improved, the problem of low solid-base content of chlorophyllium acid is solved, and its application value and use efficiency are significantly improved.

CN119684630BActive Publication Date: 2025-05-30DAHE (SHANGHAI) ECOLOGICAL TECH CO LTD
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Patent Information

Application Number
CN202510192192.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-21
Publication Date
2025-05-30
Estimated Expiration
2045-02-21

AI Technical Summary

Technical Problem

In the prior art, the solid-base content of chlorophoric acid is relatively low, making it difficult to break through the bottleneck of 55% or even 60%, limiting its application value in agriculture and industrial fields.

Method used

Hops are used as raw materials, combined with core additives SYS (including hops, taurine, salicylic acid and magnesium sulfate, etc.), and steaming and extracting, separation and concentration through the ammonium imide method to increase the solid content of chlorosulfuric acid.

Benefits of technology

The solid-base content of chlorophoric acid has been significantly improved, from 40%-53% to 56%-75% or even above 75%, enhancing its application value and use efficiency in the agricultural and industrial fields.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the fields of biochemistry, comprehensive utilization of straw resources, separation of three elements, synthetic bio-fermentation engineering and biomass energy, and discloses a high-solid-based plant-derived fulvic acid produced using hops and its production process. The present invention discloses a production process for plant-derived fulvic acid. After adding a core auxiliary agent containing hops and mixing it with ammonium sulfite, it is used as a cooking liquid medicine. After mixing the raw materials with the cooking liquid medicine, cooking, extraction, separation, and concentration are carried out to obtain a concentrated black liquid of a fulvic acid product with a high solid-based content. The present invention can increase the solid-based content or dry-based content of plant-derived fulvic acid. Among the existing similar products on the market, the solid-based content of fulvic acid is relatively high, and the detected value is generally between 47% and 57%. According to the technical solution provided by the present invention, the solid-based content of plant-derived fulvic acid exceeds 75%, and the increase amplitude exceeds 40%.
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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 production process thereof. Background Art

[0002] Humulus lupulus Humulus lupulus L. ), a perennial climbing herb of the genus Humulus in the family Cannabaceae, is distributed in regions such as Europe, northern and northeastern Asia, and eastern America. There are wild germplasm resources in northern Xinjiang, China, and it is now cultivated in various parts of China. The immature flower spikes with fruits of Humulus lupulus can be used as medicine. It tastes bitter, slightly cold, and non-toxic; it has the effects of strengthening the stomach and promoting digestion, diuresis and calming the nerves, and is mainly used to treat indigestion, abdominal distension, edema, cystitis, pulmonary tuberculosis, cough, insomnia, leprosy and other diseases. In addition, Humulus lupulus can not only be used to brew beer, but also is a good fermenting agent and has important economic uses.

[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, forestry, fruit and other wastes including straw; Straw-derived biochemical fulvic acid is a water-soluble fulvic acid obtained by the decomposition and fermentation of straw with biological agents; Mineral-derived fulvic acid refers to a small molecular weight water-soluble humic acid with an average molecular weight of 50-100, which is extracted by physical, chemical and biological methods from peat soil, lignite and weathered coal.

[0004] At present, there are mainly four categories of preparation methods for fulvic acid: extraction method, fermentation method, electrodialysis method and extraction method. The extraction method includes acid extraction, alkali extraction, acid-organic solvent extraction, and ion exchange resin method. The main method for obtaining fulvic acid from weathered coal, lignite, peat, etc. is the extraction method. The typical product representative is mineral source potassium fulvate. The main problem is that the pH is relatively high, generally pH 9-11. The fermentation method uses some industrial and agricultural waste materials, wood chips, etc. as raw materials, adds appropriate amounts of nutrients such as nitrogen, phosphorus, and potassium, first uses biological fermentation technology to react to obtain a fermentation material rich in fulvic acid, and then extracts the product rich in fulvic acid from the fermentation material through leaching. The typical product representatives of the fermentation method are bagasse molasses and yeast molasses fulvic acid. The main problem is the high salt content, and the salt content detection value of some products reaches 60%. The electrodialysis method belongs to a method of deep purification and is generally used for further processing and purification of the initial products of fulvic acid. The electrodialysis method is generally used for further processing and purification of the initial products of fulvic acid, and the limitation is the small scale of production and application. The extraction method uses ammonium bisulfite as an auxiliary agent to obtain plant-derived fulvic acid and cellulose pulp through cooking and extraction. The common limitation of the above various methods is the low solid-based content, generally 40%-60%.

[0005] The invention with the publication number CN 108772418 A discloses a cadmium and arsenic synchronous passivator for paddy soil. The passivator has a three-layer structure from the inside to the outside. Among them, the innermost layer is a hydrogen ion chemical consumption agent, the middle layer is a reaction accelerator humus-like substance, and the outermost layer is a mineralization precursor; the hydrogen ion chemical consumption agent is nitrate and peroxide; the reaction accelerator humus-like substance is one or more of peat soil, humic acid, fulvic acid, humin, fulvic acid, brown fulvic acid, and black fulvic acid; the mineralization precursor is reduced iron powder, ferrous salt and / or solid ferrous mineral. The cadmium and arsenic synchronous passivator with a three-layer film structure of the invention can be slowly released into the soil to fully synergistically play its role and effectively reduce the heavy metal cadmium and arsenic content in rice. The patent with the publication number CN 114044717 A includes the following steps: 1) Crushing and dissolving of 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 the proportioned soft water is added for dissolution; 2) Dissolution of auxiliary materials: Fish protein powder, seaweed essence, potassium fulvate, NAM inhibitor, and phosphorus activation agent are added to the reaction kettle for dissolution; 3) Mixing and stirring; 4) Subcontracting; 5) Packaging to obtain a special liquid fertilizer for cotton.

[0006] 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 fertilizer and solid fertilizer.

[0007] The fulvic acid prepared by the above method has wide applications in the fields of agriculture, animal husbandry, etc. due to its good nutritional value, natural environmental protection performance and relatively low cost. For example, fulvic acid straw plant fiber can be made into degradable mulch film (CN112239960 A), glue-free and formaldehyde-free fiberboard (CN 112025906 A), cotton straw molded lunch box (CN 112127194 A), non-wood fiber pulping and papermaking (CN 108179650 A), high-strength corrugated paper pulp (CN 111996827 A).

[0008] However, the key problem in using plant-derived fulvic acid as a renewable biochemistry raw material is how to separate its solid base content (mainly composed of cellulose, hemicellulose and lignin) with high quality to obtain raw materials for large-scale utilization for downstream conversion. As the most valuable renewable carbon resource, if the three elements of lignocellulose cannot be fully utilized, it will limit the economic efficiency and environmental friendliness of the development of biomass chemistry. Therefore, how to increase the solid base content of plant-derived fulvic acid and its application value is an important topic in this field. Summary of the Invention

[0009] 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 bottleneck and exceed 55% or even exceed 60% when using the ammonium sulfite method to produce fulvic acid products from plant raw materials.

[0010] 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 plant raw material fulvic acid. There have been many reports on the production of fulvic acid using related raw materials. The patent with publication number CN 208308727 U discloses a preparation system for fulvic acid potassium phosphite ammonium phosphate solid compound fertilizer. By granulation, potassium phosphite solution, ammonium phosphate solution and potassium fulvate solution are mixed to generate fulvic acid potassium phosphite ammonium phosphate solid compound fertilizer. The patent application with 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: the weathered coal is extracted with sodium hydroxide solution under heating conditions, and the filtered soy sauce-colored solution containing free humic acid is acidified with hydrochloric acid solution, and the filtered fulvic acid solution is added with sodium hydroxide and reacted under heating conditions, and the generated solid is dried, crushed and sieved to obtain the black crystal aquaculture synergist.

[0011] The difficulty in the process of plant-derived fulvic acid lies in finding a suitable core auxiliary agent to achieve the effect of increasing the solid base content of fulvic acid. The solid base content of fulvic acid on the market is generally 40-60%. Among them, the estimated content of ore-derived fulvic acid (potassium) is 55%; the highest content of plant-derived fulvic acid is 60%, generally 43%; the highest value of molasses fulvic acid is 60%. There is no report that the solid base content of plant-derived fulvic acid exceeds 61%.

[0012] To solve the technical bottleneck in production practice, the present invention proposes a high-solid-base-content plant-derived fulvic acid produced using hops and a production process. The production process includes:

[0013] S1, obtaining raw materials;

[0014] S2, obtaining the core auxiliary agent SYS (also known as the core agent, agent SYS, etc.);

[0015] S3, mixing the core auxiliary agent SYS with liquid ammonium sulfite (i.e., ammonium bisulfite) or solid ammonium sulfite dissolved in water as the cooking liquid;

[0016] S4, mixing the raw materials with the cooking liquid, and sequentially completing cooking extraction, separation, and concentration to obtain a high-solid-base-content concentrated dark fulvic acid liquid.

[0017] Preferably, the neutral ammonium sulfite method is adopted for cooking, with a pH of 6-9, using a non-Na ion buffer agent to obtain fibers and raw material cooking liquid; cooking at 160-180°C and keeping warm for 30-120 minutes. More preferably, the cooking temperature is 160-173°C and the holding time is 40-110 minutes.

[0018] Preferably, the addition sequence of raw materials and the core auxiliary agent, etc. can be to first dissolve the core auxiliary agent in water, and then synchronously load it into the digester with solid or liquid ammonium bisulfite and the raw materials, and charge the digester according to the set liquor ratio.

[0019] Preferably, the temperature is raised and kept warm according to the ammonium sulfite pulping process. The cooking temperature and holding time are set according to the different requirements of the raw materials and the target pulp properties.

[0020] Preferably, the total amount of the core auxiliary agent SYS used is 0.1%-10% of the weight of the raw materials, preferably 0.5%-5%, by mass percentage.

[0021] The core auxiliary agent SYS described above includes hops, magnesium sulfate, etc. Preferably, the core auxiliary agent further includes taurine. More preferably, the core auxiliary agent SYS includes hops, taurine, salicylic acid, and magnesium sulfate. For example, the core auxiliary agent contains hops plus magnesium sulfate, or hops plus taurine plus magnesium sulfate, or hops plus salicylic acid plus magnesium sulfate, or taurine plus salicylic acid plus magnesium sulfate, or hops plus taurine plus salicylic acid plus magnesium sulfate. Hops, taurine, salicylic acid, magnesium sulfate, etc. are all commercially available, and the addition amount is the percentage by weight of the dried raw materials. Among them, the addition amount of hops is not less than 0.1%, the addition amount of taurine is not less than 0.1%, the addition amount of salicylic acid is not less than 0.1%, and magnesium sulfate is 0.2% - 10%.

[0022] Salicylic acid itself is a plant growth regulator, which has the effects of increasing crop growth, increasing yield, inhibiting the natural aging and lifespan of crops, improving stress resistance, and enhancing the rooting ability of crops. Preferably, the dosage of salicylic acid in the core auxiliary agent SYS is 0.1% - 3% of the weight of the raw materials, preferably 1% - 2%. The dosage of hops is not less than 0.1% of the raw materials, preferably 0.5% - 5%, and more preferably 1% - 2%. Taurine 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. In the core medicament of the present invention, the weight of taurine is not less than 0.1% of the raw materials, preferably not less than 0.5% of the raw materials, such as 0.5% - 5%, and more preferably 0.5% - 3%, by mass percentage.

[0023] Using the production process of the present invention, the content of concentrated fulvic acid solid base in the obtained product reaches more than 55%. Preferably, the content of concentrated fulvic acid solid base reaches more than 60%, and more preferably, the content of fulvic acid solid base can reach 60 - 75%. Currently, the highest content of fulvic acid solid base in the market is less than 50%. The present invention 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 in the current market (the content of fulvic acid solid base 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, white roots, and vigorous vitality. When using the 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 in the current market.

[0024] After adding the core auxiliary agent SYS, the components of hops are retained in the plant-derived fulvic acid product produced. Preferably, the plant-derived fulvic acid finished product produced by adopting this technical solution contains fulvic acid, ammonium sulfate, ammonium sulfite (ammonium bisulfite), hops, etc.

[0025] The plant-derived fulvic acid described in the present invention is a small-molecular-weight fulvic acid obtained by sulfonating non-wood fiber biomass fiber raw materials, and its indicators are as follows: fulvic acid > 60%, preferably the fulvic acid content 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, and the proportion of the molecular weight < 180 is > 95%, pH 4 - 6. In the present invention, the detection method for the SYS component in fulvic acid adopts NMR, MS, HPLC, etc., and the detection standard refers to HG / T 5332-2018 "Humic Acid Bio-organic Fertilizer".

[0026] In the description of the present invention, the terms "comprise", "include" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including 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, the element defined by the statement "including a reference structure" does not exclude the existence of additional identical elements in the process, method, article or device including the said element. It should be noted that in this article, 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 such actual relationship or order between these entities or operations.

[0027] The beneficial effects of the present invention are as follows:

[0028] 1. Significantly increase the solid base content of plant-derived fulvic acid, from 40% - 53% to 56% - 75% or even more than 75%, and the increase rate is at least over 40%. It far exceeds the common fulvic acid products of the same kind on the market, including mineral-source fulvic acid (the solid base content of fulvic acid is 55%), molasses fulvic acid (the solid base content of fulvic acid is 60%), and the same kind of plant-derived fulvic acid (the highest solid base content of fulvic acid is 53%).

[0029] 2. The increase in the solid base content of fulvic acid improves the effective content of fulvic acid per unit weight or unit volume, reduces the transportation cost, improves the feasibility of fertilizer substitution, and can effectively promote fertilizer reduction and efficiency increase.

[0030] 3. Improve the production efficiency of plant-derived fulvic acid, with a high marginal return rate, greatly improve the production efficiency, and improve the carbon emission effect.

[0031] 4. Fulvic acid contains hops, salicylic acid, etc., which greatly enhances the comprehensive function of the plant source, forming a functional superposition of fulvic acid, hops and salicylic acid.

[0032] 5. A number of core auxiliary components such as hops, taurine, and salicylic acid that can increase the fixed-base content of plant-derived fulvic acid have been found, providing a relatively wide range of options for large-scale industrial production. Detailed implementation mode

[0033] The following will combine the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

[0034] Embodiment 1

[0035] A complete production process of plant-derived fulvic acid with a high fixed-base content is as follows:

[0036] (1) Raw materials: Use Hegang corncob xylose residue as raw materials.

[0037] (2) Medicine preparation: Preparation of SYS liquid medicine, dosage: magnesium sulfate 0.5%, hops 2%, both are solids, calculated by the mass of raw materials; Dilute the core auxiliary agent according to the ratio of 1:10 - 30 for standby;

[0038] The dosage of solid ammonium bisulfite is 30%, calculated by the mass of raw materials.

[0039] (3) Cooking method: Use intermittent rotary spherical cooking.

[0040] (4) Loading the pot:

[0041] When using solid ammonium bisulfite, the raw materials, ammonium bisulfite, and SYS liquid medicine are added and conveyed proportionally along with the conveyor belt.

[0042] When using liquid ammonium bisulfite, first form a mixed solution of SYS liquid medicine and liquid ammonium bisulfite, and then add the mixed solution and raw materials in proportion for conveying.

[0043] If using 30% solid content liquid ammonium, the water addition amount is (1 + 0.002 + 0.002 + 0.002 + 0.3) × 3.5 - 0.7 = 3.8 tons.

[0044] (5) Cooking. Heat up to 170°C and keep warm for 70 minutes.

[0045] (6) Blow-off.

[0046] (7) Solid-liquid separation. Solid-liquid separation is carried out by a conventional method. In this scheme, a screw extruder 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.

[0047] (8)Concentration of fulvic acid black liquor. The dilute fulvic acid black liquor is concentrated through multi-effect evaporation to obtain the commercial concentrated fulvic acid black liquor.

[0048] (9)Drying. The commercial concentrated fulvic acid black liquor is spray-dried to obtain the fulvic acid dry powder.

[0049] (10)Test results. It is sent to the Taiyuan Testing Center of the China Humic Acid Testing Industry Association for testing, and the test results are shown in Table 1. Among them, the fulvic acid (dry basis) is 71.4%.

[0050] Table 1 Test results of Example 1

[0051]

[0052] Solid base content = (weight of fulvic acid (FA) / total weight of plant-derived fulvic acid (dry basis)) %, mass percentage.

[0053] The above results show that the production process of the present invention can obtain a fulvic acid product with a high solid base content of fulvic acid.

[0054] Example 2

[0055] (1)Raw material: bamboo chips.

[0056] (2)Production process, the same as Example 1, except that 20% of ammonium sulfite is added.

[0057] (3)Core auxiliary agent formula: magnesium sulfate 0.5%, hops 1%.

[0058] (4)Test results: See Table 2. Among them, the fulvic acid (dry basis) is 68.6%

[0059] Table 2 Test results of Example 2

[0060]

[0061] The above results show that the production process of the present invention using bamboo chips as raw materials can also obtain a fulvic acid product with a high solid base content of fulvic acid.

[0062] Example 3

[0063] (1)Raw material: bamboo blocks.

[0064] (2)Production process, the same as Example 1.

[0065] (3)Core auxiliary agent formula: hops 1.0%, magnesium sulfate 1.0%.

[0066] (4)Test results: The solid base content of fulvic acid is 74.7%.

[0067] The above results show that the production process of the present invention can also obtain a fulvic acid product with a high fulvic acid solid base content using bamboo blocks as raw materials.

[0068] Example 4

[0069] (1) Raw materials: Reed.

[0070] (2) Production process, the same as in Example 1.

[0071] (3) Core auxiliary agent formula: 1.0% hops, 1.5% magnesium sulfate.

[0072] (4) Test results: The fulvic acid solid base content is 71.3%.

[0073] The above results show that the production process of the present invention can also obtain a fulvic acid product with a high fulvic acid solid base content using reed as raw materials.

[0074] Example 5

[0075] (1) Raw materials: Lignin sludge.

[0076] (2) Production process, the same as in Example 1.

[0077] (3) Core auxiliary agent formula: 0.5% hops, 1.0% salicylic acid, 0.5% magnesium sulfate.

[0078] (4) Test results: The fulvic acid solid base content is 71.4%.

[0079] The above results show that the production process of the present invention can also obtain a fulvic acid product with a high fulvic acid solid base content using lignin sludge as raw materials.

[0080] Example 6

[0081] (1) Raw materials: Bamboo powder.

[0082] (2) Production process, the same as in Example 1, with 20% ammonium sulfite.

[0083] (3) Core auxiliary agent formula: 0.5% hops, 0.5% salicylic acid, 0.5% magnesium sulfate.

[0084] (4) Test results: The fulvic acid solid base content is 57.0%.

[0085] The above results show that when the core medicament contains both salicylic acid and 0.5% hops, the dry base content of the obtained fulvic acid is not as good as that of the same dose of salicylic acid, nor as good as the solid base content obtained by using only hops.

[0086] Example 7

[0087] (1) Raw materials: Bamboo powder.

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

[0089] (3) Core additive formulation: 0.5% hops, 1.0% salicylic acid, 0.5% magnesium sulfate.

[0090] (4) Test result: The solid base content of fulvic acid is 65.1%.

[0091] The above results show that when the core medicament contains 1.0% salicylic acid and 0.5% hops at the same time, the dry base content of the obtained fulvic acid is not as good as that of the same dose of salicylic acid or hops.

[0092] Example 8

[0093] (1) Raw material: bamboo powder.

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

[0095] (3) Core additive formulation: 1.0% hops, 1.0% salicylic acid, 0.5% magnesium sulfate.

[0096] (4) Test result: The solid base content of fulvic acid is 68.4%.

[0097] The above results show that when the core medicament contains 1.0% salicylic acid and 1.0% hops at the same time, the dry base content of the obtained fulvic acid is not as good as that of the same dose of salicylic acid.

[0098] Example 9

[0099] (1) Raw material: bamboo powder.

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

[0101] (3) Core additive formulation: 0.5% hops, 2% salicylic acid, 0.5% magnesium sulfate.

[0102] (4) Test result: The solid base content of fulvic acid is 69.7%.

[0103] The above results show that when the core medicament contains 2.0% salicylic acid and 0.5% hops at the same time, the dry base content of the obtained fulvic acid is not as good as that of the same dose of salicylic acid.

[0104] Example 10

[0105] (1) Raw material: bamboo powder.

[0106] (2) Production process: same as in Example 1.

[0107] (3) Core additive formulation: 1.0% hops, 2% salicylic acid, 0.5% magnesium sulfate.

[0108] (4)Test result: The dry basis content of fulvic acid is 72.3%.

[0109] The above results show that the core agent contains 2.0% salicylic acid and 1.0% hops at the same time, and the dry basis content of the obtained fulvic acid is not as good as that of salicylic acid with the same dosage.

[0110] Example 11

[0111] (1)Raw material: Bamboo powder.

[0112] (2)Production process: The same as that in Example 1.

[0113] (3)Core additive formula: 0.5% hops, 3.0% salicylic acid, 0.5% magnesium sulfate.

[0114] (4)Test result: The dry basis content of fulvic acid is 70.0%.

[0115] The above results show that with the further increase of salicylic acid content in the core agent, the antagonistic effect between salicylic acid and hops weakens, and the dry basis content of the obtained fulvic acid is significantly improved compared with that in Example 7.

[0116] Example 12

[0117] (1)Raw material: Bamboo powder.

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

[0119] (3)Core additive formula: 1.0% hops, 3.0% salicylic acid, 0.5% magnesium sulfate.

[0120] (4)Test result: The dry basis content of fulvic acid is 75.8%.

[0121] The above results show that with the further increase of salicylic acid content in the core agent, even if the hops content also increases, the antagonistic effect between salicylic acid and hops weakens, and the dry basis content of the obtained fulvic acid is significantly improved.

[0122] Example 13 Comparative test (compared with Example 1)

[0123] (1)Raw material: Taking Hegang corn cob xylose residue as an example.

[0124] (2)Drug preparation: Prepare SYS liquid medicine according to the predetermined dosage. For example: 2% acetic acid, 0.5% magnesium sulfate, both are solids, calculated according to the mass of the raw material. Dilute the medicine with purified water in a volume ratio of 1:10 - 30 and set aside.

[0125] The dosage of solid ammonium sulfite (which can be abbreviated as ammonium) is 30%, calculated according to the mass of the raw material.

[0126] (3)Cooking method: Use intermittent rotary spherical cooking.

[0127] (4)Loading the pot:

[0128] 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.

[0129] 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 the proportion.

[0130] 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.

[0131] (5)Cooking. Heat up to 170°C and keep warm for 70 min.

[0132] (6)Blow-off.

[0133] (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 reverse washing is adopted to obtain dilute fulvic acid black liquor and crude cellulose pulp.

[0134] (8)Concentration of fulvic acid black liquor. The dilute fulvic acid black liquor is concentrated by multi-effect evaporation to obtain commercial concentrated fulvic acid black liquor.

[0135] (9)Drying. The concentrated fulvic acid black liquor is spray-dried to obtain fulvic acid dry powder.

[0136] (10)Test results. See Table 3.

[0137] Test index: Fulvic acid (dry basis) 51.1%.

[0138] Table 3 Comparison of test data between Example 1 and Example 13

[0139]

[0140] The results of the comparative example show that although both acetic acid and hops 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 the hops selected in the present invention, the obtained solid basis content of fulvic acid is 71.4%, and the improvement ratio reaches 40%. 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 the existing fulvic acid products.

[0141] Example 14

[0142] (1)Raw materials: Bamboo powder.

[0143] (2)Production process: same as in Example 1.

[0144] (3)Core additive formula: 0.5% hops, 0.5% taurine, 0.5% magnesium sulfate.

[0145] (4)Test result: The dry basis content of fulvic acid is 68.5%.

[0146] The above results show that when the core agent contains 0.5% hops and 0.5% taurine at the same time, the dry basis content of the obtained fulvic acid is significantly improved.

[0147] Example 15

[0148] (1)Raw material: bamboo powder.

[0149] (2)Production process: same as in Example 1.

[0150] (3)Core additive formula: 0.5% hops, 1.0% taurine, 0.5% magnesium sulfate.

[0151] (4)Test result: The dry basis content of fulvic acid is 72.7%.

[0152] The above results show that when the core agent contains 0.5% hops and 1.0% taurine at the same time, the dry basis content of the obtained fulvic acid is significantly improved, and the combination of hops and taurine can jointly promote the increase of the dry basis content of fulvic acid.

[0153] Example 16

[0154] (1)Raw material: bamboo powder.

[0155] (2)Production process: same as in Example 1.

[0156] (3)Core additive formula: 1.0% hops, 0.5% taurine, 0.5% magnesium sulfate.

[0157] (4)Test result: The dry basis content of fulvic acid is 71.6%.

[0158] The above results show that when the core agent contains 1.0% hops and 0.5% taurine at the same time, the dry basis content of the obtained fulvic acid is significantly higher than that without adding hops or taurine.

[0159] Example 17

[0160] (1)Raw material: bamboo powder.

[0161] (2)Production process: same as in Example 1.

[0162] (3)Core additive formula: 1.0% hops, 1.0% taurine, 0.5% magnesium sulfate.

[0163] (4)Detection result: The content of fulvic acid on dry basis is 72.7%.

[0164] The above results indicate that the core agent contains 1.0% hops and 1.0% taurine at the same time, and the dry basis content of the obtained fulvic acid is significantly improved compared with the case without adding hops or taurine.

[0165] Although the embodiments of the present invention have been shown and described, those of ordinary skill in the art can understand that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principle and spirit of the present invention. The scope of the present invention is defined by the claims and their equivalents.

Claims

1. A production process for producing plant-derived fulvic acid with high solid content using hops, characterized in that: The production process comprises: S1, obtain raw materials; S2, obtain the core additive SYS; S3, mixing the core additive SYS with ammonium sulfite as a cooking liquid; S4, after mixing the raw material with the cooking liquid, sequentially complete cooking, extraction, separation, and concentration to obtain a concentrated black liquor of fulvic acid with a high solid content; The high solid content plant-derived fulvic acid product refers to a plant-derived fulvic acid product in which the fulvic acid solid content is not less than 55%; The core additive SYS includes hops and magnesium sulfate. The amount of hops added is not less than 0.1% of the weight of the raw materials, and the amount of magnesium sulfate added is 0.2%-10%.

2. The production process according to claim 1, characterized in that: The neutral sulfite method is used for cooking, pH 6-9, and a sodium ion-free buffer is used to obtain fiber and raw material cooking liquid; cooking at 160-180°C and keeping warm for 30-120 minutes; in, The dosage of core additive SYS is not less than 0.5% of the raw material weight; The dosage of ammonium sulfite is 15%-35% of the weight of the raw material, by mass percentage.

3. The production process according to claim 1, characterized in that: The dosage of core additive SYS is 1%-10% of the raw material weight; The amount of hops in the core additive SYS is not less than 0.5% of the weight of the raw materials; The dosage of magnesium sulfate is 0.5%-5%, by mass percent.

4. The production process according to claim 2, characterized in that: The dosage of core additive SYS is 3%-5% of the raw material weight; The amount of hops in the core additive SYS is not less than 1% of the weight of the raw materials; The dosage of magnesium sulfate is 0.5%-2%, mass percentage; The cooking temperature range is 160-173°C.

5. The production process according to claim 1, characterized in that: The core additive SYS also includes salicylic acid, and the amount of salicylic acid added is not less than 2% of the weight of the raw material; The dosage of hops is 1%-2% of the raw material weight; The amount of magnesium sulfate added is 0.2%-5% of the weight of the raw material; The amount of ammonium sulfite added is 15%-35% of the weight of the raw material, by mass percentage.

6. The production process according to claim 1, characterized in that: The core additive SYS also includes taurine, and the amount of taurine added is not less than 0.1% of the weight of the raw material; The amount of hops added is 0.5%-5% of the weight of the raw materials; The amount of magnesium sulfate added is 0.5%-2% of the weight of the raw material; The amount of ammonium sulfite added is 20%-30% of the weight of the raw material; mass percentage.

7. A core auxiliary agent for the production process of plant-derived fulvic acid with high solid content, characterized in that: The core additive SYS contains hops and magnesium sulfate. The amount of hops added is not less than 0.1% of the weight of the raw materials, and the amount of magnesium sulfate added is 0.2%-10%, by mass percentage.

8. The use of the production process of producing plant-derived fulvic acid with high solid content using hops as claimed in claim 1, characterized in that: To produce high solid content plant-derived fulvic acid products, the weight of hops in the core additive SYS is 0.5%-5% of the raw material, and the solid content of the high solid content plant-derived fulvic acid products produced reaches more than 60%, by mass percentage.

9. The use according to claim 8, characterized in that: The plant-derived fulvic acid product with a high solid base content is used as a land conditioner or fertilizer to enhance the root and stem development of crops.

10. The use according to claim 8, characterized in that: The core additive SYS also contains salicylic acid or taurine, the amount of salicylic acid added is not less than 2% of the weight of the raw material, and the amount of taurine added is not less than 0.1% of the weight of the raw material; The solid content of the high solid content plant-derived fulvic acid products produced reaches more than 60% by mass.

Citation Information

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