阅读说明：本技术 一种液体纳米硅肥的制备方法 (Preparation method of liquid nano silicon fertilizer ) 是由 蔡小伶 颜建荣 于 2020-12-22 设计创作，主要内容包括：本发明涉及一种液体纳米硅肥的制备方法,其特征在于采用以下步骤：A、称取适量硅酸钠或硅酸钾或它们的混合物,添加到纯净水中,配制成氧化硅质量含量为2-8％的水溶液；B、将步骤A所得水溶液过阳离子树脂进行离子交换,得活性硅酸；C、将活性硅酸加入到反应釜中,添加碱液调整pH至9-12；加热至80-100℃,保温5min-2h,得纳米硅溶液；D、将纳米硅溶液过阳离子树脂进行离子交换,得酸性纳米硅溶液；E、按铝盐：酸性纳米硅溶液质量比0.01-0.5：100的比例,向酸性纳米硅溶液中加入铝盐,搅拌10min-6h,得改性纳米硅溶液；F、向改性纳米硅溶液中加入适量的碱性pH调节剂,调整pH至3-9,得液体纳米硅肥。本发明具有制备过程简单、环保,所得液体纳米硅肥具有pH值低的优点。(The invention relates to a preparation method of a liquid nano silicon fertilizer, which is characterized by comprising the following steps: A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the mass content of silicon oxide of 2-8%; B. b, passing the aqueous solution obtained in the step A through cation resin for ion exchange to obtain active silicic acid; C. adding active silicic acid into a reaction kettle, and adding alkali liquor to adjust the pH value to 9-12; heating to 80-100 deg.C, and maintaining the temperature for 5min-2h to obtain nanometer silicon solution; D. passing the nano silicon solution through cation resin for ion exchange to obtain acidic nano silicon solution; E. according to the weight ratio of aluminum salt: the mass ratio of the acidic nano silicon solution is 0.01-0.5: adding aluminum salt into the acidic nano silicon solution according to the proportion of 100, and stirring for 10min-6h to obtain a modified nano silicon solution; F. and adding a proper amount of alkaline pH regulator into the modified nano silicon solution, and regulating the pH to 3-9 to obtain the liquid nano silicon fertilizer. The preparation method has the advantages of simple preparation process and environmental protection, and the obtained liquid nano silicon fertilizer has the advantage of low pH value.)

1. A preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the mass content of silicon oxide of 2-8%;

B. b, passing the aqueous solution obtained in the step A through cation resin for ion exchange to obtain active silicic acid; the cationic resin is one of sulfonic styrene resin, sulfonic acrylic resin, carboxyl styrene resin and carboxyl acrylic resin;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding alkali liquor to adjust the pH value to 9-12; heating to 80-100 deg.C, and maintaining the temperature for 5min-2h to obtain nanometer silicon solution; the alkali liquor is one of ammonia water, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, sodium silicate aqueous solution and potassium silicate aqueous solution;

D. c, passing the nano silicon solution obtained in the step C through cation resin for ion exchange to obtain an acidic nano silicon solution;

E. according to the weight ratio of aluminum salt: the mass ratio of the acidic nano silicon solution is 0.01-0.5: adding aluminum salt into the acidic nano-silicon solution obtained in the step D according to the proportion of 100, and stirring for 10min-6h to obtain a modified nano-silicon solution; the aluminum salt is one or a mixture of ethyl aluminum, butyl aluminum, aluminum acetate, aluminum formate, aluminum oxalate and aluminum propionate;

F. adding a proper amount of alkaline pH regulator into the modified nano-silicon solution obtained in the step E, and regulating the pH to 3-9 to obtain a liquid nano-silicon fertilizer; the alkaline pH regulator is one of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, ammonia water and triethanolamine aqueous solution.

2. The method for preparing the liquid nano silicon fertilizer according to claim 1, which is characterized by comprising the following steps: the pH value in the step C is 10-11.

3. The method for preparing the liquid nano silicon fertilizer according to claim 1, which is characterized by comprising the following steps: and the heat preservation time in the step C is 10-60 min.

[ technical field ] A method for producing a semiconductor device

The invention relates to a preparation technology of a liquid nano silicon fertilizer, belonging to the technical field of fertilizer preparation.

[ background of the invention ]

Silicon is an important element for plant growth, most plants contain silicon, and particularly for plants such as rice, sugarcane and the like, the nutrition effect of silicon is considered to be inferior to that of nitrogen, phosphorus and potassium. According to related detection, when 1000 kg of rice is produced, the absorption amount of silicon dioxide reaches 150 kg, which exceeds the sum of nitrogen, phosphorus and potassium absorbed by rice. In the ash contents of six crops, namely rice, wheat, barley, soybean, hyacinth bean and fennel, oxides of 7 nutrient elements, such as silicon, phosphorus, potassium, calcium and the like, account for more than 80 percent of the ash contents, wherein silicon oxides account for 16-61.4 percent of the ash contents. The silicon fertilizer can improve soil, correct soil acidity, improve soil basicity, promote organic fertilizer decomposition and inhibit soil germs. For example, the pH value of the red soil dry land is about 4.5-5.2, and the red soil dry land is lack of organic matters and calcium and easy to harden. The application of silicon fertilizer can improve soil property, accelerate curing and is beneficial to increasing the yield of crops.

At present, common water-soluble silicon fertilizers in the market mainly comprise sodium silicate, potassium silicate, sodium peroxydisulfate, sodium metasilicate and the like, belong to quick-acting fertilizers, and have the defects of quick response and high pH value and easy corrosivity on crops.

[ summary of the invention ]

The invention aims to solve the technical problem of providing a preparation method of a liquid nano silicon fertilizer with a low pH value.

In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the mass content of silicon oxide of 2-8%;

B. b, passing the aqueous solution obtained in the step A through cation resin for ion exchange to obtain active silicic acid; the cationic resin is one of sulfonic styrene resin, sulfonic acrylic resin, carboxyl styrene resin and carboxyl acrylic resin;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding alkali liquor to adjust the pH value to 9-12; heating to 80-100 deg.C, and maintaining the temperature for 5min-2h to obtain nanometer silicon solution; the alkali liquor is one of ammonia water, sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, sodium silicate aqueous solution and potassium silicate aqueous solution;

D. c, passing the nano silicon solution obtained in the step C through cation resin for ion exchange to obtain an acidic nano silicon solution;

E. according to the weight ratio of aluminum salt: the mass ratio of the acidic nano silicon solution is 0.01-0.5: adding aluminum salt into the acidic nano-silicon solution obtained in the step D according to the proportion of 100, and stirring for 10min-6h to obtain a modified nano-silicon solution; the aluminum salt is one or a mixture of ethyl aluminum, butyl aluminum, aluminum acetate, aluminum formate, aluminum oxalate and aluminum propionate;

F. adding a proper amount of alkaline pH regulator into the modified nano-silicon solution obtained in the step E, and regulating the pH to 3-9 to obtain a liquid nano-silicon fertilizer; the alkaline pH regulator is one of sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, ammonia water and triethanolamine aqueous solution.

As a preferred embodiment of the present invention, the pH value in the step C is 10 to 11.

And the heat preservation time in the step C is 10-60 min.

According to the method, active silicic acid is prepared through ion exchange of water glass, then a nano silicon solution is obtained through a hydrothermal method, and then the stable low-pH liquid nano silicon fertilizer is obtained through aluminum modification. The silicon fertilizer has the beneficial effects of simple preparation process, low energy consumption, environmental friendliness, no pollution and low pH value, and overcomes the technical defect of high pH value of the conventional silicon fertilizer.

[ detailed description ] embodiments

The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.

Example 1:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the mass content of silicon oxide of 2%;

B. b, passing the aqueous solution obtained in the step A through cation resin for ion exchange to obtain active silicic acid; the cationic resin is a sulfostyrene resin;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding ammonia water to adjust the pH value to 9; heating to 80 deg.C, and maintaining the temperature for 5min to obtain nanometer silicon solution;

D. c, enabling the nano-silicon solution obtained in the step C to pass through sulfonic acrylic resin for ion exchange to obtain an acidic nano-silicon solution;

E. according to the weight percentage of ethyl aluminum: the mass ratio of the acidic nano silicon solution is 0.01: adding ethyl aluminum into the acidic nano silicon solution obtained in the step D according to the proportion of 100, and stirring for 10min to obtain a modified nano silicon solution;

F. and E, adding a proper amount of sodium hydroxide aqueous solution into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 3 to obtain the liquid nano silicon fertilizer.

Example 2:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the silicon oxide content of 8%;

B. b, passing the aqueous solution obtained in the step A through sulfonic acrylic resin for ion exchange to obtain active silicic acid;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding ammonia water to adjust the pH value to 12; heating to 100 ℃, and preserving heat for 2h to obtain nano silicon solution;

D. c, carrying out ion exchange on the nano silicon solution obtained in the step C through carboxyl styrene resin to obtain an acidic nano silicon solution;

E. according to the weight percentage of butyl aluminum: the mass ratio of the acidic nano silicon solution is 0.5: adding butyl aluminum into the acidic nano silicon solution obtained in the step D according to the proportion of 100, and stirring for 6 hours to obtain a modified nano silicon solution;

F. and E, adding a proper amount of potassium hydroxide aqueous solution into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 9 to obtain the liquid nano silicon fertilizer.

Example 3:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the silicon oxide content of 6%;

B. c, passing the aqueous solution obtained in the step A through carboxyl styrene resin for ion exchange to obtain active silicic acid;

C. b, adding the active silicic acid obtained in the step B into a reaction kettle, and then adding a potassium hydroxide aqueous solution to adjust the pH value to 10; heating to 90 ℃, and preserving heat for 1h to obtain nano silicon solution;

D. c, carrying out ion exchange on the nano silicon solution obtained in the step C through carboxyl acrylic resin to obtain an acidic nano silicon solution;

E. and (3) preparing an aluminum acetate: the mass ratio of the acidic nano silicon solution is 0.1: adding aluminum acetate into the acidic nano-silica solution obtained in the step D according to the proportion of 100, and stirring for 2 hours to obtain a modified nano-silica solution;

F. and E, adding a proper amount of ammonia water into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 5 to obtain the liquid nano silicon fertilizer.

Example 4:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the silicon oxide content of 6%;

B. c, passing the aqueous solution obtained in the step A through carboxyl acrylic resin for ion exchange to obtain active silicic acid;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding a sodium silicate aqueous solution to adjust the pH value to 10; heating to 95 deg.C, and maintaining the temperature for 30min to obtain nanometer silicon solution;

D. c, passing the nano silicon solution obtained in the step C through cation resin for ion exchange to obtain an acidic nano silicon solution;

E. according to the weight ratio of aluminum formate: the mass ratio of the acidic nano silicon solution is 0.08: adding aluminum formate into the acidic nano-silicon solution obtained in the step D according to the proportion of 100, and stirring for 5 hours to obtain a modified nano-silicon solution;

F. and E, adding a proper amount of triethanolamine aqueous solution into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 6 to obtain the liquid nano silicon fertilizer.

Example 5:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the silicon oxide content of 6%;

B. c, passing the aqueous solution obtained in the step A through carboxyl acrylic resin for ion exchange to obtain active silicic acid;

C. adding the active silicic acid obtained in the step B into a reaction kettle, and then adding a potassium silicate aqueous solution to adjust the pH value to 10; heating to 95 deg.C, and maintaining the temperature for 10min to obtain nanometer silicon solution;

D. c, passing the nano silicon solution obtained in the step C through cation resin for ion exchange to obtain an acidic nano silicon solution;

E. according to the weight ratio of aluminum oxalate: the mass ratio of the acidic nano silicon solution is 0.08: adding aluminum oxalate into the acidic nano-silica solution obtained in the step D according to the proportion of 100, and stirring for 5 hours to obtain a modified nano-silica solution;

F. and E, adding a proper amount of triethanolamine aqueous solution into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 6 to obtain the liquid nano silicon fertilizer.

Example 6:

a preparation method of a liquid nano silicon fertilizer is characterized by comprising the following steps:

A. weighing a proper amount of sodium silicate or potassium silicate or a mixture of the sodium silicate and the potassium silicate, and adding the sodium silicate or the potassium silicate into purified water to prepare an aqueous solution with the silicon oxide content of 5%;

B. c, passing the aqueous solution obtained in the step A through carboxyl styrene resin for ion exchange to obtain active silicic acid;

C. b, adding the active silicic acid obtained in the step B into a reaction kettle, and then adding a potassium hydroxide aqueous solution to adjust the pH value to 11; heating to 90 deg.C, and maintaining the temperature for 60min to obtain nanometer silicon solution;

D. c, carrying out ion exchange on the nano silicon solution obtained in the step C through carboxyl acrylic resin to obtain an acidic nano silicon solution;

E. according to the weight percentage of aluminum propionate: the mass ratio of the acidic nano silicon solution is 0.3: adding aluminum propionate into the acidic nano-silicon solution obtained in the step D according to the proportion of 100, and stirring for 2 hours to obtain a modified nano-silicon solution;

F. and E, adding a proper amount of ammonia water into the modified nano silicon solution obtained in the step E, and adjusting the pH value to 4 to obtain the liquid nano silicon fertilizer.