Production process of taurine-based plant-derived fulvic acid

Abstract

The invention discloses a product for producing a plant-derived fulvic acid product with high solid content by using taurine and a production process, and belongs to the fields of biochemical engineering, fermentation engineering and biorefinery and synthetic bioindustry. According to the production process of the plant-derived fulvic acid product, raw materials are cooked and separated by adopting an ammonium sulfite method to obtain fibers and fulvic acid, and after a medicament containing taurine is added, the mixture is mixed with liquid ammonium sulfite or solid ammonium sulfite dissolved by adding water to serve as cooking liquid medicine; mixing the raw materials with the cooking liquid medicine, cooking, extracting, separating and concentrating to obtain the fulvic acid concentrated black liquor with high solid content. The method provided by the invention can improve the solid content or dry content of the plant-derived fulvic acid product, the solid content detection value of the existing similar product fulvic acid in the market is generally 47-57%, and according to the technical scheme provided by the invention, the solid content of the plant-derived fulvic acid product is improved by 40-60%.

Description

Technical Field

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

[0002] Taurine itself is a plant growth regulator, which can increase crop growth, increase yield, inhibit natural aging of crops, extend the life of crops, improve stress resistance, and enhance the rooting ability of crops. However, there is no report on the use of taurine in the preparation of fulvic acid.

[0003] Fulvic acid is considered to be a plant growth activator and is one of the humic acids with a smaller molecular weight. Humic acid-based organic materials include water-soluble humic acid materials and water-insoluble humic acid materials. Water-soluble humic acid materials include water-soluble plant-derived sulfonated humic acid, water-soluble plant-derived biochemical humic acid and water-soluble mineral-derived humic acid: plant-derived sulfonated humic acid is a water-soluble low molecular weight humic acid obtained by sulfonation treatment of agricultural, forestry and fruit waste including straw; plant-derived biochemical humic acid is a water-soluble humic acid obtained by fermentation of straw with biological agents; mineral-derived humic acid refers to a water-soluble low molecular weight water-soluble humic acid extracted by physical, chemical and biological methods using peat soil, lignite and weathered coal as raw materials, with an average molecular weight of 50-100.

[0004] At present, there are four main methods for preparing fulvic acid. The extraction method includes acid extraction, alkali extraction, acid-organic solvent extraction, and ion exchange resin method. The extraction method is the main method for obtaining fulvic acid from weathered coal, lignite, peat, etc. The fermentation method uses industrial and agricultural waste materials, sawdust, etc. as the raw materials, and adds appropriate amounts of nutrients such as nitrogen, phosphorus, and potassium. First, the fermentation material rich in fulvic acid is obtained by using biological fermentation technology, and then the fulvic acid-rich product is extracted from the fermentation material by leaching. Electrodialysis is a deep purification method, which is generally used for further processing and purification of fulvic acid primary products. The extraction method uses ammonium sulfite as an auxiliary agent to obtain plant-based fulvic acid products and cellulose pulp through cooking and extraction.

[0005] The patent with announcement number CN 208308727 U discloses a system for preparing a humic acid potassium phosphite ammonium phosphate solid composite fertilizer. The humic acid potassium phosphite ammonium phosphate solid composite fertilizer can be generated by mixing a potassium phosphite solution, an ammonium phosphate solution and a potassium humate solution through granulation.

[0006] 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 a sodium hydroxide solution under heating conditions, filtered to obtain a soy sauce-colored solution containing free humic acid, the soy sauce-colored solution is then acidified with a hydrochloric acid solution, filtered to obtain a fulvic acid solution, sodium hydroxide is then added to the fulvic acid solution and reacted under heating conditions, and the generated solid is dried, crushed, and sieved to obtain the black crystal aquaculture synergist.

[0007] The patent with publication number CN 114044717 A includes the following steps: 1) crushing and dissolving inorganic raw materials: crushing the proportioned solid raw materials including urea, monoammonium phosphate, potassium tripolyphosphate, diammonium phosphate, and boric acid through a raw material crushing device, placing them in a reactor, and adding proportioned soft water for dissolution; 2) dissolving auxiliary materials: adding fish protein powder, seaweed extract, potassium humate, NAM inhibitor, and phosphorus activator into the reactor for dissolution; 3) mixing and stirring; 4) subcontracting; 5) packaging to obtain a liquid fertilizer for cotton.

[0008] The invention of publication number CN105503475A discloses a microcapsule-encapsulated amino acid liquid mineral fertilizer, which uses sodium hydroxide aqueous solution as a raw material and is obtained by producing liquid fertilizer and solid fertilizer and microencapsulating them to obtain a finished product.

[0009] However, the key difficulty in using plant-derived fulvic acid products as renewable biochemical raw materials is how to separate their solid base content (mainly cellulose, hemicellulose and lignin) with high quality to obtain raw materials for large-scale utilization for downstream conversion. In the past, chemical treatments such as acid, alkali, and organic solvents could be used to partially separate lignin, hemicellulose, and cellulose components, but usually only one or two of them (mainly cellulose) could be used, 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 increase 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 a dry state, to break through the upper limit of the currently commonly used fulvic acid content, so as to improve the application efficiency and reduce the production cost.

[0011] Increasing the solid content of fulvic acid can increase the efficacy of fulvic acid at the same 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 technical difficulty lies in finding a suitable agent to achieve the effect of increasing the solid content of fulvic acid produced by the ammonium sulfate method.

[0012] The solid content of fulvic acid refers to the content of fulvic acid in dry form. The solid content of fulvic acid on the market is generally 40%-60%, of which the estimated content of mineral fulvic acid (potassium) is 55%; plant fulvic acid products - up to 60%, generally 43%; molasses fulvic acid - the highest value is 60%.

[0013] In order to solve the technical bottleneck in production practice, the present invention proposes a technical solution for producing plant-derived fulvic acid with high solid base content, with sodium sulfite and taurine as the core.

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

[0015] The present invention uses taurine to produce a plant-derived fulvic acid product with a high solid content, and the fulvic acid stock solution obtained after concentration has a pH of 5-6 and a solid content of not less than 55% by mass. Preferably, the solid content of the concentrated fulvic acid product reaches 60%-80%.

[0016] Accordingly, the present invention provides a production process for producing a plant-based fulvic acid product with a high solid content using taurine. The order of adding the raw material components is to first dissolve the agent in water, and then load it into a digester simultaneously with the ammonium sulfite solid or liquid and the raw materials, and then load it into the pot according to the set liquid ratio.

[0017] Specifically, the production process includes: S1, obtain raw materials; S2, obtain the medicine SYS; S3, mixing the reagent SYS with liquid imine or solid imine dissolved in water to form a cooking liquid; S4, after mixing the raw material cooking liquid with the cooking liquid, sequentially complete cooking extraction, separation, and concentration to obtain a concentrated black liquid of fulvic acid with a high solid content; The medicine SYS includes taurine and magnesium sulfate; The amount of taurine added is not less than 0.1% of the weight of the raw materials, and the amount of magnesium sulfate is 0.2%-2%.

[0018] The core agent SYS (core agent is also called agent, agent SYS, etc.) includes taurine and magnesium sulfate. Specific combinations include salicylic acid plus magnesium sulfate, taurine plus magnesium sulfate, or taurine plus salicylic acid plus magnesium sulfate, etc.

[0019] Adding taurine to the core agent of the present invention 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.

[0020] The production process of using taurine to produce a high solid content plant-based fulvic acid product in the present invention adopts a neutral imine method for cooking, the pH value is 6-9, and the fiber and raw material cooking liquid is obtained. The fulvic acid stock solution obtained after concentration has a pH of 5-6 and a solid content of not less than 60%, by mass percentage. Solid content refers to the content of solids, which is different from the solid content. Here, solid content refers to the mass percentage of solid mass in the fulvic acid stock solution.

[0021] Preferably, the cooking temperature ranges from 160-180°C, more preferably from 160-175°C, such as 165°C, 168°C, 170°C, 173°C, and the like.

[0022] The insulation time ranges from 30 to 120 min, preferably from 50 to 100 min.

[0023] In the present invention, the amount of each component added in the core agent SYS is the dry weight percentage of the raw material, and the amount of the agent SYS is 1%-10% of the weight of the raw material. Preferably, the amount of the agent SYS is 3%-5% of the weight of the raw material, by mass percentage. The produced plant-derived fulvic acid product retains the component of taurine. Among them, the amount of taurine added is 0.1%-10%, preferably 0.5%-5%, 1%-5% of the weight of the raw material, and more preferably 2%-3%, for example 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 amount of taurine added is 1%.

[0024] Preferably, ammonium sulfite is added in the preparation process of the present invention, and the amount of ammonium sulfite is 15%-35% by weight of the raw material. More preferably, the amount of ammonium sulfite is 18%-35% by weight of the dry raw material. The dry raw material weight refers to the weight of the raw material converted to a dry basis.

[0025] Accordingly, the present invention provides a product of producing plant-derived fulvic acid with high solid content by using taurine. In the plant-derived fulvic acid product, the plant-derived fulvic acid product produced by the technical solution contains taurine.

[0026] In a second aspect, the present invention provides a reagent for a production process of a plant-derived fulvic acid product with a high solid content using taurine. The reagent contains taurine and magnesium sulfate; the taurine content accounts for 0.1%-10% of the raw material weight, and the magnesium sulfate content is 0.2%-2%, by mass percentage.

[0027] Preferably, the core agent of the present invention may also contain salicylic acid. The amount of salicylic acid added is not less than 0.1% of the raw material mass and not more than 3%, excluding the end value. More preferably, it is not less than 0.5%, for example, 0.5%-2.0%. Adding salicylic acid to the core agent at this concentration can further promote the increase of the fulvic acid content in the product, especially the fulvic acid content in the solid product after drying.

[0028] In a third aspect, the present invention provides an application of a production process for producing a plant-based fulvic acid product with a high solid base content using taurine. When fulvic acid is produced using the production process, the solid base content of the produced fulvic acid is not less than 57%.

[0029] The solid base content of fulvic acid products on the market is mostly less than 50%, while the solid base content of the fulvic acid product of the present invention is not less than 57%, or even higher than 60%, by mass percentage. This can greatly improve the application value and use efficiency of the product. The test of the present invention shows that compared with the fulvic acid with a higher solid base content on the market (the fulvic acid solid base content is less than 50%), the use of fulvic acid with a high solid base content significantly enhances the development of wheat root system, which is manifested as strong rhizomes, white roots and strong vitality. When a product with a fulvic acid solid base content greater than 70% is applied to wheat, the average length of the wheat root system after 20 days is nearly 3 times that of the fulvic acid with a higher solid base content on the market.

[0030] Preferably, the neutral subammonium method is adopted for cooking, pH 6-9, and a buffer without Na ions is used to obtain fiber and raw material cooking liquid; cooking is carried out at 160-173° C. and heat preservation is carried out for 30-120 minutes.

[0031] Preferably, the core agent SYS includes taurine, salicylic acid, magnesium sulfate, etc., all of which are commercially available.

[0032] Preferably, the temperature is raised and kept warm according to the ammonium sulfite pulping process. The cooking temperature and the keeping time are set according to the raw materials and the target pulp performance requirements.

[0033] Preferably, the amount of the core additive SYS is 0.1%-10% by weight of the raw material, preferably 0.5%-5%, by mass percent.

[0034] The amount of taurine in the core additive SYS is not less than 0.1% of the weight of the raw material, and more preferably not less than 1%. For example, the amount of taurine is 0.5%-10%, 1%-8%, 3%-5% and 1-2% by weight of the raw material.

[0035] 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 amount of taurine added can be 0.1-3% of the weight of the raw material, the magnesium sulfate can be 0.5%-2% of the weight of the raw material, and the content of salicylic acid can be 0.1%-3% of the weight of the raw material, by mass percentage. More preferably, the amount of taurine added is 0.5-1% of the weight of the raw material, the magnesium sulfate is 0.5%-1% of the weight of the raw material, and the content of salicylic acid is 0.5%-2% of the weight of the raw material, by mass percentage.

[0036] In the present invention, the raw materials for producing fulvic acid are selected from various plants or their wastes: one or more of corn stalks, corn cobs, lignin sludge, bamboo, reeds, cotton stalks, wheat stalks, and straw. For example, the plant-derived fulvic acid product obtained by using corn cob raw materials from Linyi has a fulvic acid content of 75.79% and a water-soluble humic acid content of 78.71%, by mass percentage. In another preferred example, bamboo chips from Jiangxi are used as raw materials, ammonium sulfite 30%, taurine 5%, and magnesium sulfate 0.5%, to obtain 71.3% fulvic acid, pH 5.6. In another preferred example, bamboo block raw materials, salicylic acid 2%, sulfite 30%, magnesium sulfate 0.5%, and taurine 1%, are used to obtain 72.7% fulvic acid.

[0037] Preferably, after adding the core auxiliary agent SYS, the taurine component is retained in the produced plant-derived fulvic acid product. Preferably, the finished 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.

[0038] The plant-derived fulvic acid product of the present invention is a low-molecular-weight fulvic acid obtained by sulfonating a non-wood fiber biomass fiber raw material, and its indicators are: fulvic acid>60%, preferably fulvic acid content greater than 75%, organic matter content 50%-70%, humic acid content 60%-70%, humic acid 0.2%-0.36%, average molecular weight <50, molecular weight <180 accounts for >95%, pH 4-6.

[0039] In the present invention, the detection method of SYS components in fulvic acid adopts NMR, MS, and HPLC. The detection standard of fulvic acid refers to HG / T 5332-2018 "Humic Acid Bio-Organic Fertilizer".

[0040] In the method of the present invention, after adding the core additive SYS, the solid base content of fulvic acid can be significantly increased by 40%, for example, from 40%-50% to 70% or even higher.

[0041] In a fourth aspect, the present invention provides a plant-derived fulvic acid product.

[0042] The core agent containing taurine is used to produce a plant-derived fulvic acid product with a high solid content. The fulvic acid stock solution obtained after concentration has a pH of 5-6 and a solid content of not less than 55%-57%, by mass percentage. Preferably, the solid content of the produced fulvic acid is not less than 60%.

[0043] The high solid content plant-derived fulvic acid product of the present invention can be used as a fertilizer, a soil conditioner, a plant growth promoter or a nutrient solution additive, etc. Plant raw materials for producing fulvic acid include, but are not limited to, one or more of corn stalks, corn cobs, lignin sludge, bamboo, reeds, cotton stalks, wheat stalks and rice straw.

[0044] In the description of the present invention, the terms "comprises", "comprising" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "comprising a reference structure" do not exclude the presence of other identical elements in the process, method, article or device comprising the elements. 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.

[0045] The beneficial effects of the present invention include: 1. Significantly increase the solid content of plant-derived fulvic acid products from 40%-50% to 60% or even more than 70%, with the lowest increase exceeding 40%. This is much higher than the common fulvic acid products on the market, including mineral-derived fulvic acid, molasses fulvic acid, and similar plant-derived fulvic acid products.

[0046] 2. The increase in the solid base content of humic acid increases the effective content of humic acid per unit weight or unit volume, reduces transportation costs, improves the feasibility of fertilizer substitution, and can effectively promote fertilizer saving and efficiency improvement.

[0047] 3. The production efficiency of plant-based fulvic acid products has been improved, with high marginal returns, which greatly improves production efficiency and carbon emission effects.

[0048] 4. The taurine contained in fulvic acid greatly enhances the comprehensive function of the plant source, forming a superposition of the functions of fulvic acid and taurine. DETAILED DESCRIPTION

[0049] The present invention provides a product and production process of plant-derived fulvic acid with high solid content using salicylic acid. The raw materials and method of a complete production process of plant-derived fulvic acid with high solid content are as follows: (1) Raw materials: Hegang corn cob xylose residue is used as raw material.

[0050] (2) Preparation: Preparation of SYS liquid medicine. The core medicine is mainly in solid form, calculated by the mass of raw materials; dilute the medicine at a ratio of 1:10-30 and set aside; Taking 30% of solid ammonium sulfite as an example, it is calculated based on the mass of raw materials.

[0051] (3) Cooking method: intermittent ball steaming.

[0052] (4) Loading the pot: When solid ammonium sulfite is used, the raw material, ammonium sulfite and SYS solution are added and transported along the conveyor belt in proportion.

[0053] When liquid ammonium sulfite is used, the SYS solution and the liquid ammonium sulfite are first mixed to form a mixed solution, and then the mixed solution and the raw materials are added and transported according to a proportion.

[0054] If liquid ammonium sulfide with a solid content of 30% is used, the amount of water added is (1+0.002+0.002+0.002+0.3)×3.5-0.7=3.8 tons.

[0055] (5) Steaming: Raise the temperature to 170°C and keep warm for 70 minutes.

[0056] (6) Spraying.

[0057] (7) Solid-liquid separation. Solid-liquid separation is carried out by conventional means. In this scheme, a screw squeezer is used to separate straw cellulose and fulvic acid black liquor, and four-stage reverse washing is used to obtain fulvic acid dilute black liquor and cellulose coarse pulp.

[0058] (8) Concentration of humic acid black liquor. The dilute humic acid black liquor is concentrated by multi-effect evaporation to obtain concentrated humic acid black liquor.

[0059] (9) Drying. The concentrated black liquor of fulvic acid is spray-dried to obtain fulvic acid dry powder.

[0060] (10)Test results.

[0061] The solid content of fulvic acid refers to the content of fulvic acid in the dry state. The fulvic acid product needs to be dried into dry powder and then the content of fulvic acid is detected and calculated. The corresponding calculation formula is: Solid base content = fulvic acid (FA) weight / total weight of plant-based fulvic acid products (dry basis), mass percentage.

[0062] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0063] Example 1 (1) Raw materials: bamboo chips.

[0064] (2) The production process is the same as the steps and methods of the above embodiment.

[0065] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 0.5% taurine.

[0066] (4) Test results: Fulvic acid (dry basis) 61.2%.

[0067] The above results show that by adding taurine to the core agent and combining it with magnesium sulfate, the solid base content of the humic acid product obtained is significantly improved by producing the plant raw materials using the ammonium sulfite method.

[0068] Example 2 (1) Raw materials: bamboo blocks.

[0069] (2) Production process: same as in Example 1.

[0070] (3) Pharmaceutical formula: 0.2% magnesium sulfate, 1% taurine.

[0071] (4) Test results: Fulvic acid (dry basis) 62.9%.

[0072] The above results show that the production process of the present invention can use not only bamboo chips as raw materials, but also bamboo blocks as raw materials. Both bamboo chips and bamboo blocks can be taken from common bamboo forests, usually as waste. The present invention uses taurine to add to the core agent, and uses the ammonium sulfite method to produce the plant raw materials that were originally waste. The solid base content of the obtained fulvic acid product is significantly improved, and it is also more environmentally friendly.

[0073] Example 3 (1) Raw material: lignin sludge.

[0074] (2) Production process: same as in Example 1.

[0075] (3) Pharmaceutical formula: 15% magnesium sulfate, 5% taurine.

[0076] (4) Test results: Fulvic acid (dry basis) 69.0%.

[0077] The above results indicate that the production process of the present invention is also applicable to lignin sludge commonly found in the land.

[0078] Example 4 (1) Raw materials: xylose residue.

[0079] (2) Production process: same as in Example 1.

[0080] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 2% taurine.

[0081] (4) Test results: Fulvic acid (dry basis) 67.5%.

[0082] The above results show that the production process of the present invention is also applicable to xylose residue.

[0083] Example 5 (1) Raw material: reed.

[0084] (2) Production process: same as in Example 1.

[0085] (3) Pharmaceutical formula: 2% magnesium sulfate, 5% taurine.

[0086] (4) Test results: Fulvic acid (dry basis) 72.9%.

[0087] The above results show that the production process of the present invention is also applicable to reeds.

[0088] Example 6 (1) Raw material: corn stalks.

[0089] (2) Production process: same as in Example 1. Imidazine 20%.

[0090] (3) Pharmaceutical formula: magnesium sulfate 0.5%, taurine 0.1%.

[0091] (4) Test results: Fulvic acid (dry basis) 41.8%.

[0092] The above results show that too low a taurine addition or a reduced amount of ammonium sulfite will result in insufficient fulvic acid content on a dry basis. Although it is also applicable and has a higher fulvic acid solid content than many similar products currently sold and used on the market, its effect still needs to be improved for use as a fertilizer or soil conditioner with high requirements.

[0093] Example 7 (1) Raw material: corn stalks.

[0094] (2) Production process: same as in Example 1, but with 20% imine.

[0095] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 0.5% taurine.

[0096] (4) Test results: Fulvic acid (dry basis) 48.0%.

[0097] The above results show that under the same amount of magnesium sulfate and ammonium sulfide added and production process conditions, increasing the amount of taurine is helpful to increase the solid base content of fulvic acid. A proportion of 0.4% of the raw material content can significantly increase the content of fulvic acid. However, in general, the joint action of core agents and related ingredients is needed to further increase the absolute amount of fulvic acid solid base content.

[0098] Example 8 (1) Raw material: corn stalks.

[0099] (2) Production process: same as in Example 1.

[0100] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 1.0% taurine.

[0101] (4) Test results: Fulvic acid (dry basis) 64.0%.

[0102] The above results show that increasing the dosage of taurine is helpful to improve the solid base content of fulvic acid. The proportion of taurine in the raw material content of 1.0% can significantly increase the content of fulvic acid - more than 60%. Compared with the fulvic acid products with a higher content of 45%-50% on the market, the solid base content of fulvic acid in the present invention is increased by more than 20%.

[0103] Example 9 (1) Raw material: corn stalks.

[0104] (2) Production process: same as in Example 1.

[0105] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 3.0% taurine.

[0106] (4) Test results: Fulvic acid (dry basis) 70.6%.

[0107] The above results show that under the same amount of magnesium sulfate and ammonium sulfide added and production process conditions, increasing the amount of taurine is helpful to increase the solid base content of fulvic acid. The proportion of taurine in the raw material content of 3.0% can make the fulvic acid content exceed 70%. Compared with the fulvic acid products with a higher content of 45%-50% on the market, the fulvic acid solid base content of the present invention is increased by more than 40%.

[0108] Example 10 (1) Raw material: corn stalks.

[0109] (2) Production process: same as in Example 1.

[0110] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 5% taurine.

[0111] (4) Test results: Fulvic acid (dry basis) 75.7%.

[0112] The above results show that increasing the amount of taurine helps to increase the solid content of fulvic acid, and the proportion of taurine in the raw material content of 5.0% can make the content of fulvic acid exceed 75%. Compared with the 45%-50% fulvic acid products with a higher content on the market, the fulvic acid solid content of the present invention is increased by 50% or more, but compared with the case of lower taurine content, after taurine accounts for 5.0% of the raw material content, the further taurine content on the fulvic acid solid content The ratio of the increase is not as obvious as before.

[0113] Embodiment 11 (1) Raw material: corn stalks.

[0114] (2) Production process: same as in Example 1.

[0115] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 0.5% salicylic acid, and 0.1% taurine.

[0116] (4) Test results: Fulvic acid (dry basis) 73.4%.

[0117] The above results show that in the presence of taurine, adding salicylic acid can increase the solid content of fulvic acid.

[0118] Example 12 (1) Raw material: corn stalks.

[0119] (2) Production process: same as in Example 1.

[0120] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 1.0% salicylic acid, 0.5% taurine.

[0121] (4) Test results: Fulvic acid (dry basis) 75.3%.

[0122] The above results show that in the presence of taurine, adding salicylic acid can increase the solid content of fulvic acid. However, significantly increasing the content of taurine or salicylic acid does not further significantly increase the solid content of fulvic acid as expected.

[0123] Embodiment 13 (1) Raw material: corn stalks.

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

[0125] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 1% salicylic acid, and 1% taurine.

[0126] (4) Test results: Fulvic acid (dry basis) 72.6%.

[0127] The above results show that in the presence of taurine, adding salicylic acid can increase the solid content of fulvic acid. However, significantly increasing the content of taurine or salicylic acid does not further significantly increase the solid content of fulvic acid as expected. Moreover, this example further increases the content of taurine, but the dry basis content of fulvic acid is not further increased.

[0128] Embodiment 14 (1) Raw material: corn stalks.

[0129] (2) Production process: same as in Example 1.

[0130] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 2% salicylic acid, 0.5% taurine.

[0131] (4) Test results: Fulvic acid (dry basis) 75.8%.

[0132] The above results show that in the presence of high dosages of taurine and salicylic acid, further increasing salicylic acid does not significantly increase the solid base content of fulvic acid as expected.

[0133] Embodiment 15 (1) Raw material: corn stalks.

[0134] (2) Production process: same as in Example 1.

[0135] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 2% salicylic acid, and 1.0% taurine.

[0136] (4) Test results: Fulvic acid (dry basis) 72.5%.

[0137] The above results show that when taurine and salicylic acid are already present in high dosages, adding salicylic acid and taurine at the same time does not further significantly increase the solid content of fulvic acid as expected. Instead, it may lead to a decrease in the solid content of fulvic acid in the fulvic acid product.

[0138] Example 16 (1) Raw material: corn stalks.

[0139] (2) Production process: same as in Example 1.

[0140] (3) Pharmaceutical formula: 0.5% magnesium sulfate, 3% salicylic acid, 0.5% taurine.

[0141] (4) Test results: Fulvic acid (dry basis) 73.3%.

[0142] Embodiment 17 (1) Raw material: corn stalks.

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

[0144] (3) Pharmaceutical formula: magnesium sulfate 1.0%, taurine 0.5%.

[0145] (4) Test results: Fulvic acid (dry basis) 72.0%.

[0146] The results of Examples 16 and 17 show that in the presence of relatively high amounts of taurine and salicylic acid, further increasing salicylic acid may instead result in a slight decrease in the solid-base fulvic acid content in the fulvic acid product.

[0147] Comparative Example Compared with Example 1, fulvic acid was produced using corncob xylose residue as raw material.

[0148] (1) Raw materials: Take Hegang corn cob xylose residue as an example.

[0149] (2) Preparation: Prepare SYS solution according to the predetermined dosage, for example: 2% acetic acid, 0.5% magnesium sulfate, both solid, calculated by the mass of raw materials. Dilute the agent with clean water at a volume ratio of 1:10-30 and set aside.

[0150] The amount of solid ammonium sulfite (which may be referred to as ammonium sulfite for short) used is 30%, calculated based on the mass of the raw materials.

[0151] (3) Cooking method: intermittent ball steaming.

[0152] (4) Loading the pot: When solid ammonium sulfite is used, the raw material, ammonium sulfite and SYS solution are added and transported along the conveyor belt in proportion.

[0153] When liquid ammonium sulfite is used, the SYS solution and the liquid ammonium sulfite are first mixed to form a mixed solution, and then the mixed solution and the raw materials are added and transported according to a proportion.

[0154] If liquid ammonium sulfide with a solid content of 30% is used, the amount of water added is (1+0.002+0.002+0.002+0.3)×3.5-0.7=3.8 tons.

[0155] (5) Steaming: Raise the temperature to 170°C and keep warm for 70 minutes.

[0156] (6) Spraying.

[0157] (7) Solid-liquid separation. Solid-liquid separation is carried out in a conventional manner. In this scheme, a screw squeezer is used to separate straw cellulose and fulvic acid black liquor. Four-stage reverse washing is used to obtain fulvic acid dilute black liquor with a solid content of 16% and cellulose coarse pulp.

[0158] (8) Concentration of fulvic acid black liquor. The 16% fulvic acid dilute black liquor is concentrated by multi-effect evaporation to obtain commercial fulvic acid concentrated black liquor with a solid content of 55% (volume concentration).

[0159] (9) Drying. The concentrated black liquor of humic acid with a solid content of 55% is spray-dried to obtain humic acid dry powder.

[0160] (10)Test results.

[0161] Detection indicators: fulvic acid (dry basis) 51.08%, water-soluble humic acid content 54.65%, carboxyl 0.26 (ad mmol / g), phenolic hydroxyl 0.08 (ad mmmol / g).

[0162] The results of the comparative example show that although both acetic acid and taurine can be used in the production of fulvic acid products, the dry basis content of the obtained fulvic acid is also high. However, after the same amount of acetic acid is added, the obtained fulvic acid solid base content is 51.1%, while after the addition of taurine selected by the present invention, the obtained fulvic acid solid base content is 67.4%, and the increase ratio reaches 32%. Whether the high solid base fulvic acid product is used for fertilizer, improving soil texture or other purposes, it has higher efficiency and lower cost than existing fulvic acid products.

[0163] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A taurine-based plant-derived fulvic acid production process, characterized in that: The production process comprises: S1, obtain raw materials; S2, obtain the medicine SYS; S3, mixing the reagent SYS with ammonium sulfite as a cooking liquid; S4, after mixing the raw material cooking liquid with the cooking liquid, sequentially completing cooking, extraction, separation, and concentration to obtain a concentrated black liquid of fulvic acid with a high solid content; The medicine SYS includes taurine and magnesium sulfate; The amount of taurine added is not less than 0.1% of the weight of the raw material, and the amount of magnesium sulfate added is 0.2%-2% of the weight of the raw material, by mass percentage.

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

3. The taurine-based plant-derived fulvic acid production process according to claim 1, characterized in that: The dosage of the agent SYS is 1%-10% of the weight of the raw material, and the amount of taurine added is 1%-5% of the weight of the raw material, by mass percentage; The plant raw materials are steamed by neutral ammonium sulfite method, and the pH value is 6-9 to obtain fiber and raw material steaming liquid. The humic acid stock solution obtained after concentration has a pH of 5-6 and a solid content of not less than 55% by mass; The cooking temperature range is 160-180°C, and the insulation time range is 30-120min.

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

5. The taurine-based plant-derived fulvic acid production process according to claim 1, characterized in that: The amount of ammonium sulfite used is 20%-30% of the weight of the raw material on a dry basis, and the amount of taurine used in the agent SYS is 1%-3% of the weight of the raw material, by mass percentage.

6. The taurine-based plant-derived fulvic acid production process according to claim 1, characterized in that: The amount of taurine added is not less than 0.5% of the weight of the raw material, and the amount of magnesium sulfate added is 0.5%-2% of the weight of the raw material, by mass percentage.

7. The taurine-based plant-derived fulvic acid production process according to claim 1, characterized in that: The medicament also contains salicylic acid, and the content of salicylic acid is no more than 3%.

8. The process for producing 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 process for producing taurine-based plant-derived fulvic acid according to claim 7, characterized in that: The amount of taurine added is 0.1%-3% of the weight of the raw material, the amount of magnesium sulfate added is 0.5%-2% of the weight of the raw material, and the amount of salicylic acid added is 0.1%-3% of the weight of the raw material, in mass percentage.

10. The taurine-based plant-derived fulvic acid production process according to claim 7, characterized in that: The amount of taurine added is 0.5-1% of the weight of the raw material, the amount of magnesium sulfate added is 0.5%-1% of the weight of the raw material, and the amount of salicylic acid added is 0.5%-2% of the weight of the raw material, in mass percentage.