阅读说明：本技术 一种黄腐植酸盐水溶肥的生产方法 (Production method of fulvic acid salt water-soluble fertilizers ) 是由 林晓山 于 2019-09-08 设计创作，主要内容包括：本发明公开了一种黄腐植酸盐水溶肥的生产方法。该生产方法包括配置饱和溶肥、酸化反应、碱化反应、络合反应、螯合反应、研磨与熟化、过滤与检测等步骤。本发明利用生产蔗糖产生的废糖蜜生产黄腐植酸钾和矿物型腐植酸盐的水溶肥；解决废糖蜜生产其他产品废物排放污染自然环境、破坏生态平衡问题,同时还可以产生良好的经济效益。(The invention discloses a production method of kinds of fulvic acid salt water-soluble fertilizers, which comprises the steps of preparing saturated soluble fertilizers, carrying out acidification reaction, alkalization reaction, complexing reaction, chelation reaction, grinding and curing, filtering, detecting and the like.)

The production method of the water-soluble fertilizer of the yellow humate of varieties is characterized by comprising the following steps:

1) preparing a saturated dissolved fertilizer: preparing a sodium hydroxide saturated solution;

2) and (3) acidification reaction: adding the waste molasses into a reaction tank, adding deionized water under the condition of stirring, uniformly stirring, adding potassium dihydrogen phosphate, mixing and acidifying; continuously stirring for reacting for 20-40 min, adding 85% phosphoric acid, and continuously acidifying, and measuring pH of the reaction solution to be less than or equal to 3.5 after the phosphoric acid is basically dissolved;

3) alkalization reaction: adding the potassium hydroxide saturated solution obtained in the step 1) into the reaction tank obtained in the step 2) for reaction to obtain potassium fulvate;

4) and (3) complexing reaction: adjusting the pH value of the reaction system in the step 3) to be less than or equal to 7, and adding the crushed urea under the condition of continuous stirring; in the dissolving process of urea, mixing and dissolving amino acid, citric acid and magnesium sulfate to prepare a mixed solution, then adding the mixed solution into a reaction system, and stirring to continue carrying out a complex reaction;

5) carrying out chelation reaction: stirring, mixing and dissolving the trace elements, the chelating agent, the citric acid and the deionized water, adding the mixture into the reaction system in the step 4), uniformly mixing, stirring, adding the mineral potassium humate and the dispersing agent in the continuous reaction process, carrying out chelation reaction for 20-28 hours, adding the auxin solution, and continuously stirring for reaction;

6) grinding and curing: transferring the product obtained after the chelation reaction in the step 5) into a grinder for grinding, and stirring and curing for 2-4 days after grinding to obtain a crude product of the fulvic acid salt water-soluble fertilizer;

7) and (3) filtering and detecting: filtering the coarse product of the fulvic acid salt water-soluble fertilizer obtained in the step 6) by using a belt-free vacuum filter, and detecting technical indexes of the filtrate to obtain qualified filtrate, namely the fulvic acid salt water-soluble fertilizer.

2. The production method of the fulvic acid salt water-soluble fertilizer according to claim 1, wherein the addition amounts of the waste molasses, the deionized water, the monopotassium phosphate and the phosphoric acid with the mass concentration of 85% in the step 2) are as follows in parts by weight: 100-150 parts of waste molasses, 80-120 parts of deionized water, 80-120 parts of monopotassium phosphate and 50-70 parts of phosphoric acid with the mass concentration of 85%.

3. The method for producing the fulvic acid salt water-soluble fertilizer as set forth in claim 1, wherein the amount of saturated potassium hydroxide in the step 3) is 150-200 parts by weight.

4. The method for producing the fulvic acid salt water-soluble fertilizer as set forth in claim 1, wherein the amounts of urea, magnesium sulfate, citric acid and amino acid used in step 4) are respectively 280 parts by weight of urea, 45-55 parts by weight of amino acid, 5-10 parts by weight of citric acid and 8-15 parts by weight of magnesium sulfate.

5. The method for producing the fulvic acid salt water-soluble fertilizer according to claim 4, wherein the reaction time in the step 4) is controlled to be 50-70 minutes.

6. The production method of the fulvic acid salt water-soluble fertilizer according to claim 1, wherein the trace elements in step 5) include Fe, Cu, B, Zn, Mg and Mo, which are added in the form of copper sulfate, magnesium sulfate, manganese sulfate, ferrous sulfate, boric acid and ammonium molybdate respectively, and the addition amounts are 0.8-1.2 parts by weight respectively; the dosage of the chelating agent is 1.2 to 1.8 weight parts; the addition amount of the mineral potassium humate is 45-55 parts by weight; the addition amount of the dispersant is 3-8 parts by weight.

7. The method for producing the fulvic acid salt water-soluble fertilizer according to claim 6, wherein the chelating agent is EDTA and the dispersing agent is polyethylene glycol.

8. The method for producing the fulvic acid salt water-soluble fertilizer according to claim 1, wherein times of stirring are carried out every 3-5 hours in the curing process in the step 6), and the stirring time is 30-60 minutes.

Technical Field

The invention belongs to the technical field of recycling of sugar industry waste materials, and particularly relates to a production method of types of fulvic acid salt water-soluble fertilizers.

Background

With the development of scientific technology, scientific fertilization is also promoted in agriculture to save fertilizing amount and improve the utilization rate of fertilizers, and water-saving agriculture with water and fertilizers is promoted in many places due to uneven water resource distribution in China.

At present, of waste molasses is used for producing caramel pigment, monosodium glutamate and fermented alcohol (most common fermented alcohol production), besides little pollution to the environment caused by production of caramel pigment, the pollution to the environment caused by waste water of other products is serious, especially the pollution to the waste liquid after alcohol production by waste molasses is serious, the treatment process is a world problem, biochemical, physical and chemical and biogas fermentation has been used, water dilution and irrigation have been used to cause soil hardening, and seepage influences underground water quality.

The southern Yunnan, west, east and Hainan provinces in China are large provinces of cane sugar, about 6000 million tons of cane sugar are produced each year, the waste molasses is calculated according to 2.5-3% of the cane sugar amount, 150 million tons/ years, all the waste molasses are used as organic water-soluble fertilizers, 300 million tons of fulvic acid organic water-soluble fertilizers can be produced each year according to 4 tons of concentrated solution, 6 million tons/year of potash fertilizers can be recycled, 1.8 million tons/year of nitrogenous fertilizers and 0.75 million tons/year of phosphatic fertilizers, and China is used as a large agricultural country and has great demand for fertilizers each year, but due to the lack of potash fertilizer resources, a great amount of imports are needed each year, and a great amount of financial and material resources are consumed.

However, there are not effective methods for processing waste molasses produced in sugar industry into fulvic acid water-soluble fertilizer.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention aims to provide methods for producing fulvic acid salt by using waste molasses alcohol waste liquid, and the method is used for producing potassium fulvic acid and mineral type humate water-soluble fertilizer by using waste molasses produced in sucrose production, solves the problems that waste discharge of other products produced by waste molasses pollutes the natural environment and destroys the ecological balance, and can also produce good economic benefit.

In order to solve the problems, the technical scheme adopted by the invention is as follows:

the production method of kinds of fulvic acid salt water-soluble fertilizer comprises the following steps:

1) preparing a saturated dissolved fertilizer: preparing a sodium hydroxide saturated solution;

2) and (3) acidification reaction: adding the waste molasses into a reaction tank, adding deionized water under the condition of stirring, uniformly stirring, adding potassium dihydrogen phosphate, mixing and acidifying; continuously stirring for reacting for 20-40 min, adding 85% phosphoric acid, and continuously acidifying, and measuring pH of the reaction solution to be less than or equal to 3.5 after the phosphoric acid is basically dissolved;

3) alkalization reaction: adding the potassium hydroxide saturated solution obtained in the step 1) into the reaction tank obtained in the step 2) for reaction to obtain potassium fulvate;

4) and (3) complexing reaction: adjusting the pH value of the reaction system in the step 3) to be less than or equal to 7, and adding the crushed urea under the condition of continuous stirring; in the dissolving process of urea, mixing and dissolving amino acid, citric acid and magnesium sulfate to prepare a mixed solution, then adding the mixed solution into a reaction system, and stirring to continue carrying out a complex reaction;

5) carrying out chelation reaction: stirring, mixing and dissolving the trace elements, the chelating agent, the citric acid and the deionized water, adding the mixture into the reaction system in the step 4), uniformly mixing, stirring, adding the mineral potassium humate and the dispersing agent in the continuous reaction process, carrying out chelation reaction for 20-28 hours, adding the auxin solution, and continuously stirring for reaction;

6) grinding and curing: transferring the product obtained after the chelation reaction in the step 5) into a grinder for grinding, and stirring and curing for 2-4 days after grinding to obtain a crude product of the fulvic acid salt water-soluble fertilizer;

7) and (3) filtering and detecting: filtering the coarse product of the fulvic acid salt water-soluble fertilizer obtained in the step 6) by using a belt-free vacuum filter, and detecting technical indexes of the filtrate to obtain qualified filtrate, namely the fulvic acid salt water-soluble fertilizer.

As a scheme of step , in the production method, the adding amounts of the waste molasses, the deionized water, the potassium dihydrogen phosphate and the phosphoric acid with the mass concentration of 85% in the step 2) are respectively 150 parts by weight of the waste molasses, 80-120 parts by weight of the deionized water, 80-120 parts by weight of the potassium dihydrogen phosphate and 50-70 parts by weight of the phosphoric acid with the mass concentration of 85%.

As a means for the step , in the production process of the present invention, the amount of the saturated potassium hydroxide in the step 3) is 150-200 parts by weight.

As a scheme of the step , in the production method, the amounts of the urea, the magnesium sulfate, the citric acid and the amino acid in the step 4) are respectively 280 parts of the urea, 45-55 parts of the amino acid, 5-10 parts of the citric acid and 8-15 parts of the magnesium sulfate in parts by weight.

As a means for the step , in the production process of the present invention, the reaction time in the step 4) is controlled to 50 to 70 minutes.

, in the production method, the trace elements in the step 5) comprise Fe, Cu, B, Zn, Mg and Mo, and are added in the forms of copper sulfate, magnesium sulfate, manganese sulfate, ferrous sulfate, boric acid and ammonium molybdate respectively, wherein the addition amounts are respectively 0.8-1.2 parts by weight, the dosage of the chelating agent is 1.2-1.8 parts by weight, the addition amount of the mineral potassium humate is 45-55 parts by weight, and the addition amount of the dispersing agent is 3-8 parts by weight.

In the production method of the present invention, as the step , the chelating agent is EDTA, and the dispersant is polyethylene glycol.

As a scheme of step , in the production method, in the curing process of step 6), stirring is carried out for times every 3-5 hours, and the stirring time is 30-60 minutes.

Compared with the prior art, the invention has the beneficial effects that:

1. the production method of the fulvic acid salt water-soluble fertilizer can be used for efficiently utilizing the waste molasses generated after cane sugar production to produce the fulvic acid salt water-soluble fertilizer, so that the economic benefit is improved, and the problems of environmental pollution and the like are solved;

2. the production method of the fulvic acid salt water-soluble fertilizer solves the problem that the natural ecological balance is damaged by the waste water discharge in the sugar industry, protects the huge measures of ocean, rivers and lake water flows, utilizes the waste liquid to produce the water-soluble fertilizer, and improves the utilization rate of inorganic fertilizer; greatly reducing the damage of inorganic fertilizer to the soil, ensuring good cultivation conditions of the soil, overcoming the import requirements of a large amount of chemical fertilizers and the like;

3. when the fulvic acid salt water-soluble fertilizer obtained by the production method is applied to planting vegetables, the plant diseases and insect pests and the limit content of the vegetables can be effectively reduced; when the fertilizer is used for planting fruits, fruit cracking and fruit dropping can be effectively prevented, and the yield of the fruits is improved; during the fertilization of the land, the pH value of the land can be effectively changed, the land is prevented from hardening, and the soil changing function is realized.

The present invention is further described in with reference to specific embodiments.

Detailed Description

The production method of the fulvic acid salt water-soluble fertilizer comprises the following steps:

1) preparing a saturated dissolved fertilizer: preparing a sodium hydroxide saturated solution;

2) and (3) acidification reaction: adding the waste molasses into a reaction tank, adding deionized water under the condition of stirring, uniformly stirring, adding potassium dihydrogen phosphate, mixing and acidifying; continuously stirring for reacting for 20-40 min, adding 85% phosphoric acid, and continuously acidifying, and measuring pH of the reaction solution to be less than or equal to 3.5 after the phosphoric acid is basically dissolved;

3) alkalization reaction: adding the potassium hydroxide saturated solution obtained in the step 1) into the reaction tank obtained in the step 2) for reaction, wherein the reaction is exothermic reaction, the reaction temperature cannot be more than or equal to 50 ℃, and the reaction time is 8 hours, so as to obtain the potassium fulvate;

4) and (3) complexing reaction: adjusting the pH value of the reaction system in the step 3) to be less than or equal to 7, and adding the crushed urea under the condition of continuous stirring; in the dissolving process of urea, mixing and dissolving amino acid, citric acid and magnesium sulfate to prepare a mixed solution, then adding the mixed solution into a reaction system, and stirring to continue carrying out a complex reaction;

5) carrying out chelation reaction: stirring, mixing and dissolving the trace elements, the chelating agent, the citric acid and the deionized water, adding the mixture into the reaction system in the step 4), uniformly mixing, stirring, adding the mineral potassium humate and the dispersing agent in the continuous reaction process, carrying out chelation reaction for 20-28 hours, adding the auxin solution, and continuously stirring for reaction;

6) grinding and curing: transferring the product obtained after the chelation reaction in the step 5) into a grinder for grinding, and stirring and curing for 2-4 days after grinding to obtain a crude product of the fulvic acid salt water-soluble fertilizer;

7) and (3) filtering and detecting: filtering the coarse product of the fulvic acid salt water-soluble fertilizer obtained in the step 6) by using a belt-free vacuum filter, and detecting technical indexes of the filtrate to obtain qualified filtrate, namely the fulvic acid salt water-soluble fertilizer.

As a scheme of step , in the production method, the adding amounts of the waste molasses, the deionized water, the potassium dihydrogen phosphate and the phosphoric acid with the mass concentration of 85% in the step 2) are respectively 150 parts by weight of the waste molasses, 80-120 parts by weight of the deionized water, 80-120 parts by weight of the potassium dihydrogen phosphate and 50-70 parts by weight of the phosphoric acid with the mass concentration of 85%.

As a means for the step , in the production process of the present invention, the amount of the saturated potassium hydroxide in the step 3) is 150-200 parts by weight.

As a scheme of the step , in the production method, the amounts of the urea, the magnesium sulfate, the citric acid and the amino acid in the step 4) are respectively 280 parts of the urea, 45-55 parts of the amino acid, 5-10 parts of the citric acid and 8-15 parts of the magnesium sulfate in parts by weight.

In the research of the present invention, it was found that the reaction time can be controlled to effectively prevent the ammonia volatilization due to the decomposition of urea at an excessively high pH, and therefore, as a further alternative to step , the reaction time in step 4) of the production method of the present invention is controlled to be 50 to 70 minutes, preferably 60 minutes.

, in the production method, the trace elements in the step 5) comprise Fe, Cu, B, Zn, Mg and Mo, and are added in the forms of copper sulfate, magnesium sulfate, manganese sulfate, ferrous sulfate, boric acid and ammonium molybdate respectively, wherein the addition amounts are respectively 0.8-1.2 parts by weight, the dosage of the chelating agent is 1.2-1.8 parts by weight, the addition amount of the mineral potassium humate is 45-55 parts by weight, and the addition amount of the dispersing agent is 3-8 parts by weight.

As a scheme of step , in the production method, the chelating agent is EDTA and the dispersing agent is polyethylene glycol.

, the production method comprises the step 6) of curing, wherein stirring is carried out for times every 3-5 hours for 30-60 minutes, and the stirring in the grinding and curing process aims to ensure that various substances are distributed more uniformly without generating precipitates and ensure that the water-soluble fertilizer is cured more uniformly.

The following are specific examples of the present invention, and the raw materials, reagents, and equipment used in the following examples are commercially available.