CN106380321A - Compound fertilizer antiblocking agent, and preparation and application methods thereof - Google Patents

Abstract

The invention discloses an anti-caking agent for compound fertilizer, the components of which include (mass percentage): 40.0-70.0% of vegetable oil, 10.0-30.0% of paraffin, 1.0-10.0% of stearic acid, 1.0-10.0% of octadecylamine, Vinyl acetate 1.0~10.0%, surfactant 1.0~10.0%, benzoyl peroxide 0.02~0.20%. After the compound fertilizer anti-caking agent in the present invention is mixed with the compound fertilizer, a composite film with stronger moisture-proof and waterproof ability than the existing anti-caking agent can be formed on the surface of the compound fertilizer, and the film can effectively prevent environmental moisture Intrusion, thereby preventing the compound fertilizer particles from sticking to each other into agglomerates. In addition, the slow-release performance of the compound fertilizer after mixing will be significantly improved, and finally the fertilizer efficiency of the compound fertilizer will be improved. The invention also provides a preparation method of the compound fertilizer anti-caking agent and a method of using the compound fertilizer anti-caking agent.

Description

A kind of anti-caking agent for compound fertilizer and its preparation and use method

technical field

The invention belongs to the technical field of compound fertilizer anti-caking treatment, and in particular relates to a compound fertilizer anti-caking agent and a preparation and use method thereof.

Background technique

Affected by environmental factors such as moisture, temperature, and stacking pressure, compound fertilizers tend to agglomerate easily, which is not only inconvenient for the storage and transportation of compound fertilizers, but also causes great troubles for fertilization. Therefore, whether compound fertilizer can effectively prevent caking has become an important indicator for people to evaluate the quality of fertilizer.

Existing compound fertilizer anti-caking agents have three types: powder type, water-solvent type and oil-soluble type: 1. The powder type anti-caking agent uses inert powder to block the formation of crystal bridges between fertilizer particles, but it needs to be sprayed into the oily type at the same time. Substances adhere to inert powders. Although this method has an anti-coagulation effect, the process is complicated, the cost is high, and the fertilizer dust is increased. 2. The water-solvent anti-caking agent is to dissolve the surfactant in water and spray it on the surface of the fertilizer to reduce the surface tension of the fertilizer and play an anti-caking effect. The disadvantage of this method is that it brings in moisture, which is the direct cause of fertilizer caking. 3. The oil-solvent anti-caking agent avoids the shortcomings of the above two methods, and has the advantages of convenient use and good effect. However, the traditional method needs to add mineral oil (such as engine oil) as a solvent, and the amount of mineral oil is large. The amount of mineral oil in a ton of compound fertilizer reaches 2-3kg, and these mineral oils are difficult to degrade when they enter the soil with the fertilizer, causing a certain degree of pollution to the soil and the surrounding environment.

CN101555178A discloses an anti-caking agent for fertilizers, the components of which include (mass percentage): 5-20% of dodecafluoroheptanol succinate sulfonate, containing primary amine salts or secondary amines with 6-40 carbon atoms 9-30% of amine salt, 10-50% of phospholipid oil, 10-40% of fatty acid ester, 5-30% of fatty acid, 1-20% of paraffin, and the sum of each component is 100%.

CN101798248A discloses a special anti-caking agent for nitro compound fertilizer, its preparation method and application. %, industrial wax oil 13-50%, fatty acid ester 10-40%, fatty acid amide 5-30%, paraffin 1-20%, dihexadecafluorononyl succinic acid monoester amine salt 4-8%.

CN101870607A discloses a fully biodegradable compound fertilizer/compound fertilizer anti-caking agent, which consists of fatty acids, anionic surfactants, cationic surfactants, polyether polymer surfactants and fatty acid esters, each component The mass percentages are: fatty acid 84.5%-90%, anionic surfactant 2%-3%, cationic surfactant 0.2%-1%, polyether polymer surfactant 0.5%-1.5%, fatty acid ester 5% %-10%.

CN102070373A discloses a degradable compound fertilizer anti-caking agent, the components and mass percentage of which are: 10-20% of fatty amine or its salt, 20-25% of stearic acid, 15-20% of oleic acid, 5-20% of refined glycerin 15%, waste edible oil 20-50%, the sum of each component is 100%.

CN104355819A discloses a degradable compound fertilizer anti-caking agent, its components include fatty amine or its salt, stearic acid, oleic acid, refined glycerin, waste edible oil, the sum of the above-mentioned components is 100%, wherein , each component is proportioned according to the following percentages: fatty amine or its salt: 5-15%, stearic acid: 15-20%, oleic acid: 10-14%, refined glycerin: 5-15%, waste edible oil: 20-50%.

In summary, the commonly used surfactant types are: anionic surfactants, mainly alkyl sulfates, alkylbenzene sulfonates, a-olefin sulfonates, etc.; cationic surfactants, mainly quaternary ammonium salt surfactants ; Nonionic surfactants, mainly polyoxyethylene fatty alcohol, polyoxyethylene alkylphenol, polyoxyethylene fatty acid amide, PO-EO block copolymer, polyoxyethylene polyoxypropylene glycerol, polyoxyethylene fatty acid , polyoxyethylene alkylamine, polyoxyethylene sorbitan fatty acid ester, etc.; amphoteric surfactant, etc.

However, the anti-caking agent in the above-mentioned prior art still mainly depends on the film-forming effect of fatty acid (ester) and fatty (amide) amide for its moisture-proof and waterproof function and conjunctiva, although other organic substances added have certain hydrophobicity, but The overall effect of moisture-proof and waterproof is not ideal all the time. In addition, the slow-release performance of the fertilizer mixed with the above-mentioned anti-caking agent is not ideal.

Contents of the invention

The technical problem to be solved by the present invention is to overcome the deficiencies and defects mentioned in the above background technology, and provide a kind of anti-caking performance, which is green and environmentally friendly; after mixing with fertilizer, the slow-release performance of fertilizer is significantly improved, which is convenient for fertilizer Anti-caking agent for compound fertilizer absorbed by crops.

In order to realize the above-mentioned invention object, the present invention provides a kind of compound fertilizer anti-caking agent, is made up of vegetable oil, paraffin, stearic acid, surfactant, octadecylamine, vinyl acetate, benzoyl peroxide, each component The mass percentage composition is as follows: vegetable oil: 40.0~70.0%; paraffin wax: 10.0~30.0%; stearic acid: 1.0~10.0%; octadecylamine: 1.0~10.0%; vinyl acetate 1.0~10.0%; surfactant: 1.0 ~10.0%; Benzoyl peroxide: 0.02~0.20%, the sum of the above components is 100%.

Further, the mass percentages of the above components can be preferably: vegetable oil: 50.0~65.0%; paraffin: 13.0~23.0%; stearic acid: 4.0~9.0%; octadecylamine: 4.0~9.0%; 8.0%; surfactant: 3.0~8.0%; benzoyl peroxide: 0.05~0.10%, the sum of the above components is 100%.

The vegetable oil is any one or a mixture of any two or more of palm oil, rapeseed oil, peanut oil, coconut oil, camellia oil, and edible vegetable oil recovery oil, and any two or more of them are mixed in any proportion .

The paraffin is liquid paraffin, solid paraffin, or a mixture of liquid paraffin and solid paraffin in any proportion.

Preferably, the surfactant is a nonionic surfactant or an anionic surfactant.

Preferably, the anionic surfactant is an alkylbenzene sulfonate.

Preferably, the nonionic surfactant is Span-60, Span-80, Tween-60, Tween-80.

The present invention also provides a kind of method for preparing above-mentioned compound fertilizer anti-caking agent, it comprises the steps:

(1) Melting: Take the paraffin, stearic acid and octadecylamine in the stated ratio, heat them with steam to 60-65° C. and stir to make them fully melt to obtain the melted mixture I;

(2) Fusion: Continue to heat the mixture I at a temperature of 65-70°C, add the vegetable oil and surfactant in the stated ratio, and mix evenly to obtain the mixture II;

(3) To mixture II, first add vinyl acetate in the stated proportion, then add benzoyl peroxide, and stir for 30 min to 60 min at a temperature of 65 to 80°C to obtain the anti-coagulation compound fertilizer blocks.

The present invention also provides a method for using the above compound fertilizer anti-caking agent, the prepared compound fertilizer anti-caking agent within 2h,

At 70~85°C, use high-pressure spraying method to mix compound fertilizers. Preferably, high-pressure spraying immediately after compound fertilizer anti-caking agent is synthesized has a better effect. The dosage of compound fertilizer anti-caking agent is 1.5‰～3.0‰ of the compound fertilizer weight.

In the present invention, benzoyl peroxide is added to trigger the controllable and directional self-polymerization of vinyl acetate, the self-polymerization of unsaturated fatty acids in vegetable oils, and the cross-polymerization of vinyl acetate and unsaturated fatty acids in vegetable oils, thereby forming polysaccharides. A structured polymer film. And the film molecules formed by stearic acid and octadecylamine are inserted into these polymers to form a new type of composite film with interpenetrating network structure, which not only effectively improves the moisture-proof and waterproof ability of the anti-caking agent, but also reflects better Anti-caking effect, and make the wrapped fertilizer have a better slow-release effect.

Compared with prior art, principle of the present invention and beneficial effect thereof are:

(1) Under the catalysis of benzoyl peroxide, vinyl acetate undergoes self-polymerization reaction in the system to form a controllable and directional polyvinyl acetate film with low degree of polymerization, so as to improve the moisture-proof and waterproof ability of the anti-caking agent ;

(2) Utilize unsaturated fatty acids in vegetable oils under the catalysis of benzoyl peroxide to undergo self-polymerization in the system to form a controllable, low-polymerization and degradable polymeric grease film to improve the moisture-proof and waterproof ability of the anti-caking agent ;

(3) Under the catalysis of benzoyl peroxide, the unsaturated fatty acid and vinyl acetate in vegetable oil undergo cross-polymerization reaction in the system to form a mixed film of polyvinyl acetate and polymerized oil with interpenetrating network structure. To synergize the moisture-proof and waterproof effect, improve the moisture-proof and waterproof ability;

(4) Utilize the film-forming effect of stearic acid and octadecylamine itself, and after they enter polyvinyl acetate film, polymerized grease film and interpenetrating polyvinyl acetate and polymerized grease mixed film, the resulting A special type of film that acts as a synergistic moisture-proof and waterproof effect;

(5) Due to the occurrence of various chemical reactions in the anti-caking agent system, various types of composite films with interpenetrating network structures are formed, which not only synergistically improves the moisture-proof and waterproof effects, but also forms several types of films with biological properties. Degradability, will not cause harm to the soil. In addition, the compound fertilizer wrapped in it will make its fertilizer effect release slowly, thus improving the long-term effect of fertilizer.

detailed description

In order to facilitate the understanding of the present invention, the invention will be described more comprehensively and in detail below in conjunction with the diagrams of the description and preferred embodiments, but the protection scope of the present invention is not limited to the following specific embodiments.

Unless otherwise defined, all technical terms used hereinafter have the same meanings as commonly understood by those skilled in the art. The terminology used herein is only for the purpose of describing specific embodiments, and is not intended to limit the protection scope of the present invention.

Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

Example 1

A compound fertilizer anti-caking agent, the mass percent of each component is:

Rapeseed Oil: 65.0%; Solid Paraffin: 13.0%; Stearic Acid: 5.0%; Stearylamine: 9.0%; Span-80: 3.45%; Vinyl Acetate: 4.5%; Benzoyl Peroxide: 0.05% . The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the solid paraffin, stearic acid and octadecylamine in the stated ratio, add them to the reaction kettle with a stirring device, heat them with steam to 65°C, make them fully melt and react, and obtain the melted mixture ;

(2) Fusion: continue to heat the above melted mixture to 70°C, add the vegetable oil and Span-80 in the stated proportion, and after mixing, add the vinyl acetate in the stated proportion, and then add the stated proportion benzoyl peroxide, and stirred at 75°C for 40 min to obtain an anti-caking agent for compound fertilizer.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above is heated to about 80° C. after 1.5 hours, and the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer is 1.8‰, and the high-pressure spraying method is carried out.

Comparative example 1

According to the proportioning ratio of Example 1, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the compound fertilizer anti-caking agent are the same as in Example 1.

Example 2

A compound fertilizer anti-caking agent, the mass percent of each component is:

Palm oil: 20.0%, rapeseed oil 25.0%; solid paraffin: 5.0%, liquid paraffin: 15.0%; stearic acid: 10.0%; octadecylamine: 9.0%; Span-60: 8.4%; vinyl acetate: 7.5%; Benzoyl Peroxide: 0.10%. The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the paraffin wax, stearic acid and octadecylamine in the stated ratio, add them into a reaction kettle with a stirring device, heat them with steam to 60°C, make them fully melt and react, and obtain a melted mixture;

(2) Fusion: continue to heat the above melted mixture to 70°C, add the vegetable oil and Span-60 in the stated proportion, and after mixing, add the vinyl acetate in the stated proportion, and then add the stated proportion benzoyl peroxide, and stirred at 75°C for 35 minutes to obtain an anti-caking agent for compound fertilizer.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above was treated by high-pressure spraying at about 75°C after 1 hour, according to the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer being 2.0‰.

Comparative example 2

According to the proportioning ratio of Example 2, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the compound fertilizer anti-caking agent are the same as in Example 2.

Example 3

A compound fertilizer anti-caking agent, the mass percent of each component is:

Palm Oil: 35%, Rapeseed Oil 15.0%; Liquid Paraffin: 13.0%; Solid Paraffin: 13.0%; Stearic Acid: 5.0%; Stearylamine: 5.0%; Tween-80: 7%; Vinyl Acetate: 6.85%; Benzoyl Peroxide: 0.15%. The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the paraffin wax, stearic acid and octadecylamine in the stated proportions, add them into a reaction kettle with a stirring device, heat them with steam to 65°C, make them fully melt and react, and obtain a melted mixture;

(2) Fusion: continue to heat the above melted mixture to 70°C, add the vegetable oil and Span-80 in the stated proportion, and after mixing, add the vinyl acetate in the stated proportion, and then add the stated proportion benzoyl peroxide, and stirred at 80°C for 30 minutes to obtain an anti-caking agent for compound fertilizer.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above is immediately processed by high-pressure spraying at about 70° C., according to the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer being 2.5‰.

Comparative example 3

According to the proportioning ratio of Example 3, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the anti-caking agent for compound fertilizer are the same as in Example 3.

Example 4

A compound fertilizer anti-caking agent, the mass percent of each component is:

Palm oil: 35%, rapeseed oil 15.0%; liquid paraffin: 13.0%; solid paraffin: 13.0%; stearic acid: 5.0%; octadecylamine: 5.0%; sodium dodecylbenzenesulfonate: 7% ; Vinyl Acetate: 6.85%; Benzoyl Peroxide: 0.15%. The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the paraffin wax, stearic acid and octadecylamine in the stated proportions, add them into a reaction kettle with a stirring device, heat them with steam to 65°C, make them fully melt and react, and obtain a melted mixture;

(2) Fusion: continue to heat the above-mentioned melted mixture to 70°C, add the vegetable oil and alkylbenzene sulfonate in the stated proportion, and after mixing, add the vinyl acetate in the stated proportion, and then add the Benzoyl peroxide in the above ratio was incubated and stirred at 80° C. for 30 minutes to obtain a compound fertilizer anti-caking agent.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above is immediately processed by high-pressure spraying at about 70° C., according to the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer being 2.5‰.

Comparative example 4

According to the proportioning ratio of embodiment 4, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the compound fertilizer anti-caking agent are the same as in embodiment 4.

Example 5

A compound fertilizer anti-caking agent, the mass percent of each component is:

Palm Oil: 35%, Rapeseed Oil 15.0%; Liquid Paraffin: 13.0%; Solid Paraffin: 13.0%; Stearic Acid: 5.0%; Stearylamine: 5.0%; Tween-60: 7%; Vinyl Acetate: 6.85%; Benzoyl Peroxide: 0.15%. The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the paraffin wax, stearic acid and octadecylamine in the stated proportions, add them into a reaction kettle with a stirring device, heat them with steam to 65°C, make them fully melt and react, and obtain a melted mixture;

(2) Fusion: continue to heat the above-mentioned melted mixture to 70°C, add the vegetable oil and polyoxyethylene polyoxypropylene glycerol in the stated proportion, and then add the vinyl acetate in the stated proportion after mixing evenly. Then add the benzoyl peroxide in said ratio, keep stirring at 80° C. for 30 minutes, and obtain the compound fertilizer anti-caking agent.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above is immediately processed by high-pressure spraying at about 70° C., according to the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer being 2.5‰.

Comparative example 5

According to the proportioning ratio of Example 5, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the compound fertilizer anti-caking agent are the same as in Example 5.

Example 6

A compound fertilizer anti-caking agent, the mass percent of each component is:

Palm oil: 35%, rapeseed oil 15.0%; liquid paraffin: 13.0%; solid paraffin: 13.0%; stearic acid: 5.0%; stearylamine: 5.0%; Span-60: 7.0%; vinyl acetate: 6.85%; Benzoyl Peroxide: 0.15%. The sum of the above components is 100%.

The preparation method of described compound fertilizer anti-caking agent is as follows:

(1) Melting: Take the paraffin wax, stearic acid and octadecylamine in the stated ratio, add them into a reaction kettle with a stirring device, heat them with steam to 65° C., make them fully melt and react, and obtain a melted mixture;

(2) Fusion: continue to heat the above melted mixture to 70°C, add the vegetable oil and Tween-60 in the stated proportion, and after mixing, add the vinyl acetate in the stated proportion, and then add the stated proportion benzoyl peroxide, and stirred at 80°C for 30 minutes to obtain an anti-caking agent for compound fertilizer.

The using method of described compound fertilizer anti-caking agent is as follows:

The compound fertilizer anti-caking agent prepared above is immediately treated by high-pressure spraying at about 70° C., according to the weight ratio of the weight of the anti-caking agent: the weight of the compound fertilizer being 2.5‰.

Comparative example 6

According to the proportioning ratio of Example 6, but without adding vinyl acetate and benzoyl peroxide, the preparation and use method of the compound fertilizer anti-caking agent are the same as in Example 6.

Determination and comparison of anti-caking effect

The compound fertilizer containing the compound fertilizer anti-caking agent prepared in each of Examples 1 to 6 and Comparative Examples 1 to 6 was formed into a cylinder of Φ50×70 mm under a pressure of 2 MPa, and then placed under this pressure 80% relative humidity, temperature 60 ℃ test box for 12 hours, and then placed in 60% relative humidity, temperature 40 ℃ test box under this pressure for 12 hours, so cycled 5 times, and then placed at room temperature for 24 hours, to get the sample . Then the sample falls freely from a height of 1m onto the ground platform, and then sieves the sample with an industrial sieve (aperture 5mm) for 1min, weighs the sieve residue, and calculates the agglomeration rate according to the following formula.

Agglomeration rate (%) = sieve residue / sample weight × 100%

Table 1 is the comparison experiment result of embodiment 1～6 and comparative example 1～6.

Table 1: a list of comparative experimental results of the caking rate of the anti-caking agent of the embodiment and the comparative example

Example number Add ratio* Agglomeration rate** Comparative scale number add ratio Agglomeration rate Example 1 1.8‰ 2.8% Comparative example 1 1.8‰ 16.5% Example 2 2.0‰ 2.0% Comparative example 2 2.0‰ 13.8% Example 3 2.5‰ 0.0% Comparative example 3 2.5‰ 5.6% Example 4 2.5‰ 0.9% Comparative example 4 2.5‰ 8.2% Example 5 2.5‰ 1.7% Comparative example 5 2.5‰ 11.4% Example 6 2.5‰ 1.1% Comparative example 6 2.5‰ 8.8%

Addition ratio*: mass ratio of anti-caking agent/compound fertilizer; **caking rate: average value of three experiments.

Experiments show that: the addition of vinyl acetate and benzoyl peroxide in the embodiment can significantly reduce the caking rate of the compound fertilizer, fully meeting the requirements of the compound fertilizer on the anti-caking rate. It can be seen that the anti-caking agent of the present invention has better anti-caking effect.

Claims (9)

1. a kind of compound fertilizer anticaking agent is it is characterised in that its component includes：Vegetable oil, paraffin, stearic acid, octadecylamine, surface Activating agent, vinyl acetate, benzoyl peroxide, the mass percent composition of each component is as follows：Vegetable oil：40.0 ~ 70.0%, Paraffin：10.0 ~ 30.0%, stearic acid：1.0 ~ 10.0%, octadecylamine：1.0 ~ 10.0%, vinyl acetate：1.0 ~ 10.0.%, surface Activating agent：1.0 ~ 10.0%, benzoyl peroxide：0.02 ~ 0.20%, that above each group is divided and be 100%.

2. compound fertilizer anticaking agent according to claim 1 it is characterised in that described vegetable oil be palm oil, rapeseed oil, Peanut oil, coconut oil, tea oil, edible after vegetable oil oil recovery in any one or any two kinds and above mixing, Any two kinds and mixed above when be any proportioning.

3. compound fertilizer anticaking agent according to claim 1 is it is characterised in that described paraffin is atoleine, solid stone Wax or the mixture of atoleine and any proportioning of solid paraffin.

4. compound fertilizer anticaking agent according to claim 1 is it is characterised in that described surfactant is non-ionic surface Activating agent or anion surfactant.

5. compound fertilizer anticaking agent according to claim 4 is it is characterised in that described anion surfactant is alkyl Benzene sulfonate.

6. compound fertilizer anticaking agent according to claim 4 is it is characterised in that described nonionic surfactant is department Disk -60, Arlacel-80, Tween-60, Tween-80.

7. a kind of preparation method of compound fertilizer anticaking agent as described in any one in claim 1-6 is it is characterised in that main Comprise the steps：

(1) melt：Take paraffin, stearic acid and the octadecylamine of described ratio, be steam heated to 60 ~ 65 DEG C and stir, be allowed to fill Divide and melt, the mixture I after being melted；

(2) merge：Under 65 ~ 70 DEG C of temperature conditionss, continue heating mixture I, by the vegetable oil of described ratio and surface Activating agent is added thereto, and mixes, and obtains mixtures II；

(3) toward in mixtures II, it is initially charged the vinyl acetate of described ratio, be subsequently adding the benzoyl peroxide first of described ratio Acyl, under 65 ~ 80 DEG C of temperature conditionss, stirs 30 min ~ 60 min, obtains described compound fertilizer anticaking agent.

8. a kind of using method of compound fertilizer anticaking agent as described in any one in claim 1-6 it is characterised in that：Institute State in 2h after the completion of prepared by compound fertilizer anticaking agent, under 70 DEG C ~ 85 DEG C temperature conditionss, be allowed to using high-pressure fog mode and multiple Hefei mixes.

9. according to claim 8 the using method of compound fertilizer anticaking agent it is characterised in that the use of compound fertilizer anticaking agent Measure 1.5 ‰～3.0 ‰ for composite fertilizer's weight.