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Neutral and meta-acidic sulfonated potassium fulvate and preparation method thereof

A technology for sulfonating potassium fulvic acid and potassium humate, which is applied in the field of chemical technology, can solve problems such as adverse effects on crops, and achieve the effects of strong anti-electrolyte flocculation performance, environmental safety, and simple process

Inactive Publication Date: 2021-02-26
张坤
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even if there is a small amount of neutral potassium fulvic acid, it is neutralized with traditional inorganic acid (sulfuric acid, hydrochloric acid), which contains a large amount of Cl - or SO 4 2- ions, which can also adversely affect some crops

Method used

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  • Neutral and meta-acidic sulfonated potassium fulvate and preparation method thereof

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preparation example Construction

[0023] Such as figure 1 Shown, a kind of neutral and slightly acidic potassium sulfonated fulvic acid and preparation method thereof, preparation method comprises:

[0024] (1) Humic acid extraction: Add water, low-grade coal, KOH (or K 2 CO 3 ), react at 80-100°C for 1-3 hours, centrifuge, remove insoluble residues, and obtain potassium humate (HA-K) solution;

[0025] (2) Sulfonation of humic acid: add sulfonating agent to potassium humate (HA-K) solution, stir and react at 80-100°C for 2-4 hours, and centrifuge to obtain sulfonated potassium humate (SHA-K) solution;

[0026] (3) Neutralization of sulfonated humic acid potassium (SHA-K) solution: Add low-molecular-weight organic acid to the sulfonated humic acid potassium (SHA-K) solution under stirring to make the pH of the solution reach neutral or slightly acidic, and centrifuge Separate to obtain sulfonated fulvic acid potassium (SFA-K) solution and sulfonated brown black humic acid potassium precipitate.

Embodiment 1

[0028] Add 70L of water to the stainless steel reactor, start the agitator, add 10kg of Yunnan Zhaotong lignite powder and 1.4kg of KOH in turn, heat to 90°C, react for 2h, put the material into a centrifuge, and centrifuge at 3000r / min for 20min to remove insoluble residue , 52.3L of potassium humate (HA-K) solution was obtained, and 5.4kg of total humic acid in the solution was measured. Transfer the solution to the reactor, add K 2 SO 3 1.2kg, react at 100°C for 3h, and then centrifuge at 3000r / min for 20min to obtain sulfonated humic acid (SHA-K) solution. Slowly add 1.6 kg of tartaric acid to the SHA-K solution under stirring to make the pH of the solution = 7.0. After centrifugation, 43.5 L of sulfonated fulvic acid potassium (SFA-K) solution was obtained. The solution was evaporated and dried to obtain 4.3kg of solid SFA-K. The SFA-K product was pulverized, and its components were determined to be: moisture 6.7%, fulvic acid (FA) 67.2%, total humic acid 78.8%, pH 6...

Embodiment 2

[0030] The operation process is basically the same as in Example 1, but the sulfonating agent is changed to 1.3 kg of sodium metabisulfite, the neutralizing agent is changed to 1.6 g of citric acid, and finally the solution is dried to obtain 4.6 kg of solid SFA-K. The SFA-K product was pulverized, and its components were determined to be: moisture 5.8%, fulvic acid (FA) 70.9%, total humic acid 85.2%, pH 7.1, water insoluble matter 0.5%, K 2 O 15.7%.

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Abstract

The invention provides neutral and meta-acidic sulfonated potassium fulvate and a preparation method thereof, aiming at the urgent demand of preparing a high-end fulvic acid water-soluble fertilizer at present. The preparation method comprises the following steps: extracting, sulfonating, neutralizing and separating, and evaporating and drying when necessary. According to the invention, a potassium-containing reagent is adopted as an extracting agent and a sulfonating agent, extraction is carried out under alkalescence, low-molecular-weight organic acid is used for neutralizing until the pH value is 5.5-7.5, the obtained product does not contain inorganic ions such as Na<+>, Cl<->, SO4<2-> and the like, and a new product with high potassium, high fulvic acid, high sulfonation degree, low molecular weight, low pH value and low cost is prepared. The product is good in water solubility and strong in electrolyte flocculation resistance, and is a high-quality base material for preparing high-end water-soluble fertilizers. The method is free of waste, and precipitates after reaction can be used as raw materials of organic fertilizers and other products. The preparation method has the advantages of cheap and easily available raw materials, simple process, safety to environment and human body, easy realization of industrialization, and popularization and application in the field of modern organic agriculture.

Description

technical field [0001] The invention belongs to the field of chemical technology, and in particular relates to a production technology of neutral-slightly acidic sulfonated potassium fulvic acid. Background technique [0002] Potassium fulvic acid is an important plant growth regulator and nutrient synergist. It is currently mainly used as an organic potassium fertilizer and a basic material for the preparation of humic acid water-soluble fertilizers. In order to further improve the hydrophilicity, exchange capacity, complex water solubility and anti-electrolyte flocculation of potassium fulvic acid, it is generally necessary to increase the sulfonation step. The so-called sulfonation is a chemical reaction that introduces sulfonic acid groups into humic acid or fulvic acid molecules. This is also an important technical measure for the current preparation of cement water reducer, coal water slurry dispersant, oil drilling fluid treatment agent, water purification agent and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 张坤
Owner 张坤
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