Formula of picric acid ferrous fuel additive

Abstract

The invention discloses a formula of a picric acid ferrous fuel additive, and relates to the technical field of fuel additives, and the formula comprises the following steps: mixing aromatic hydrocarbon and fatty alcohol according to a mass ratio of 1: 9-9: 1 to prepare an anhydrous or low-water solvent system; then aromatic hydrocarbon picrate or aromatic ether picrate is added to react with the activated iron powder, and the activated iron powder is prepared by treating the activated iron powder with hydrochloric acid for 30 seconds and then cleaning the treated activated iron powder with water and alcohol; continuously reacting at the temperature of 10-80 DEG C, preferably 30-60 DEG C, so as to increase the generation amount of picric acid ferrous iron; and finally, filtering unreacted iron powder, and blending to obtain a finished product. The water content of the finished product is lower than 100 ppm, the iron content is 400 ppm, the free picric acid content is 0.4%, and the solvent is 85% toluene and 15% 2-propanol. According to the method, explosive dry picric acid is replaced with safe raw materials, the reaction is performed under the anhydrous or low-water condition, the product safety and stability are improved, the reaction time is shortened, the production efficiency is improved, the method is suitable for various fuels, and the fuel performance can be effectively improved.

Description

Technical Field

[0001] The invention relates to the technical field of fuel additives, in particular to a formula of ferrous picrate fuel additive. Background Art

[0002] Since the 1940s, ferrous picrate / picric acid-based fuel additives have been widely used in the technical field and can be used in alcohol-based fuels, gasoline, diesel and other fuels to improve fuel economy, enhance power, reduce emissions, etc. However, there are many problems with its manufacture and use. The traditional process requires excessive picric acid to maintain an acidic environment, resulting in highly corrosive, toxic and environmentally harmful products. The residues after leakage or volatilization of the carrier solvent are prone to explosion and will also corrode copper-containing alloys. At the same time, the liquid formula has poor stability and is easily degraded by moisture, and the problem is more serious during high-temperature storage and transportation. In the prior art, direct iron-

[0003] The picric acid reaction requires a high amount of water to maintain the reaction rate, but water will accelerate product deterioration. In addition, dry picric acid is explosive and reacts slowly, which hinders its industrial application.

[0004] In view of this, this application is hereby filed. Summary of the invention

[0005] The object of the present invention is to provide a formulation of ferrous picrate fuel additive to solve the problems mentioned in the above background technology.

[0006] In order to solve the above technical problems, the formula of ferrous picrate fuel additive provided by the present invention is prepared by the following steps:

[0007] Step 1: preparing a solvent mixture: mixing aromatic hydrocarbons and aliphatic alcohols in a mass ratio of 1:9-9:1 to obtain an anhydrous or low-water solvent system to obtain product 1 (solvent mixture);

[0008] Step 2: Producing ferrous picrate intermediate: adding one or both of aromatic hydrocarbon picrate and aromatic ether picrate to the product 1 (solvent mixture) obtained in step 1, and then adding activated iron powder to obtain product 2. The activated iron powder is prepared by washing the iron activated by hydrochloric acid with water and alcohol in turn to obtain a mixture containing ferrous picrate;

[0009] Step 3: Synthesis and crude product: Allow product 2 to continue to react for a period of time at 10-80° C. to make the reaction more complete and further increase the amount of ferrous picrate produced to obtain product 3 (a crude ferrous picrate mixture);

[0010] Step 4: Refining and preparation of finished products: Filter the product 3 obtained in step 3 to remove the unreacted iron powder to obtain product 4 (finished product of ferrous picrate fuel additive).

[0011] Furthermore, in step 1, the aromatic hydrocarbons are one or more of benzene, toluene, xylene, and mixed aromatic hydrocarbons.

[0012] Furthermore, in step 1, the fatty alcohol is one or more of methanol, ethanol, propanol, butanol, and C5 to C8 alcohols.

[0013] Furthermore, in step 2, the aromatic hydrocarbon picrate is one or more of benzene picrate, toluene picrate, xylene picrate, and naphthalene picrate.

[0014] Furthermore, in the step 2, the aromatic ether picrate is one or more of anisole picrate and diphenyl ether picrate.

[0015] Furthermore, in the step 2, the acid used in the acid activation treatment is hydrochloric acid, and the treatment time is 30 seconds.

[0016] Furthermore, in the step 3, the reaction temperature is preferably 30-60° C. This temperature range is conducive to a more complete reaction of the product 2 and further increases the amount of ferrous picrate produced.

[0017] Furthermore, in step 4, the moisture content of product 4 (finished product of ferrous picrate fuel additive) is less than 100 ppm, the iron content is 400 ppm, the free picric acid content is 0.4%, and the solvent is composed of 85% toluene and 15% 2-propanol.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. Improve safety: Replacing dry picric acid with non-explosive aromatic hydrocarbon / ether picrates avoids friction or impact sensitivity and reduces the risk of explosion. Reducing or eliminating moisture in the formula avoids the risk of explosion caused by leakage of the carrier solvent or dry residues after volatilization, and also reduces corrosion to copper-containing alloys.

[0020] 2. Enhanced stability: The use of water-free or low-water formula significantly improves the stability and shelf life of the product under harsh transportation and storage conditions, solves the problem of easy deterioration of traditional liquid formulas, and reduces problems such as fuel filter blockage and equipment downtime caused by product degradation.

[0021] 3. Improve reaction efficiency: Anhydrous reaction allows high temperature operation and the use of high-concentration picric acid, shortening the reaction time to 5-15 minutes. At the same time, it avoids moisture-induced deterioration and improves production efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 Flowchart for the preparation of a formulation for ferrous picrate fuel additive. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. 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.

[0024] See also Figure 1 The present invention provides a technical solution: a formula of ferrous picrate fuel additive is prepared by the following steps:

[0025] 1. Preparation of experimental materials

[0026] 1. Aromatic hydrocarbons: prepare benzene, toluene and xylene for the preparation of solvent mixture, and ensure that their purity meets the experimental requirements.

[0027] 2. Fatty alcohols: Select methanol, ethanol, propanol, and butanol as another component of the solvent system and perform purity tests on them to ensure the accuracy of the experimental results.

[0028] 3. Picrates: Benzene picrate, toluene picrate, naphthalene picrate, anisole picrate and diphenyl ether picrate were synthesized by the methods of alcohol co-solvent, azeotropic dehydration and mixed solvent method mentioned in the article, and their purity and structure were characterized by melting point determination, infrared spectroscopy analysis and other means.

[0029] 4. Iron powder: Use -200 mesh high surface area iron powder for subsequent activation treatment and reaction.

[0030] 5. Hydrochloric acid: Use analytical grade hydrochloric acid with a concentration of 12N for the activation treatment of iron powder.

[0031] 6. Other reagents: Prepare appropriate amounts of water, methanol, ethanol, etc. for cleaning iron powder, as well as inert gases such as nitrogen used during the experiment.

[0032] 2. Experimental Equipment Preparation

[0033] 1. Reaction vessel: Choose a glass reactor with a stirring device, thermometer, and condenser to ensure temperature control and uniform mixing of materials during the reaction process. The material of the reactor must be corrosion-resistant to adapt to the chemical environment in the experiment.

[0034] 2. Filtration device: Equipped with a vacuum filtration device, including a Buchner funnel, a suction filtration bottle, etc., to filter out unreacted iron powder to ensure the purity of the product.

[0035] 3. Heating device: Use an oil bath or heating jacket to accurately control the reaction temperature within the range of 10-80°C, providing suitable temperature conditions for the reaction.

[0036] 4. Testing instruments: prepare infrared spectrometer, atomic absorption spectrometer, moisture meter, etc. to detect and analyze the composition, structure and moisture content of the product.

[0037] 3. Specific implementation steps

[0038] (I) Preparation of solvent mixture

[0039] 1. Weigh appropriate amounts of aromatic hydrocarbons and fatty alcohols in a mass ratio of 1:9-9:1. For example, weigh 85g toluene and 15g 2-

[0040] Propanol was added into the reaction kettle.

[0041] 2. Turn on the stirring device and control the stirring speed at 200-300 rpm to fully mix the aromatic hydrocarbons and fatty alcohols to form a uniform anhydrous or low-water solvent system to obtain product 1 (solvent mixture).

[0042] (II) Formation of ferrous picrate intermediate

[0043] 1. Preparation of activated iron powder:

[0044] Weigh a certain amount of iron powder, place it in a beaker, add 12N hydrochloric acid at a ratio of 5-10 mL of hydrochloric acid per gram of iron powder, and activate for 30 seconds.

[0045] The activated iron powder is quickly poured into a large amount of cold water for quenching, and then rinsed three times with deionized water, each time using 10-20 times the mass of the iron powder, to remove residual hydrochloric acid.

[0046] Then, the mixture was rinsed three times with anhydrous ethanol, each time using an amount of 5-10 times the mass of the iron powder, to further remove moisture and obtain activated iron powder.

[0047] 2. Reaction to generate intermediates:

[0048] A certain amount of aromatic hydrocarbon picrate or aromatic ether picrate, such as 10 g of toluene picrate, is added to a reaction kettle containing product 1 (solvent mixture).

[0049] Then add activated iron powder, the amount of iron powder added is based on the molar ratio of picrate to iron powder of 1:1.5-2, turn on the stirring device, adjust the stirring speed to 300-500 rpm, and mix the materials thoroughly to obtain product 2 (a mixture containing ferrous picrate).

[0050] (III) Synthesis and crude products

[0051] 1. Raise the temperature of the reactor to 30-60°C, for example, set the temperature to 50°C, and use oil bath heating to raise the temperature. The heating rate is controlled at 5-10°C / min.

[0052] 2. Allow product 2 to continue to react at the temperature for 10-15 minutes, and continue stirring during the reaction at a stirring speed of 300-500 rpm to make the reaction more complete and further increase the amount of ferrous picrate produced to obtain product 3 (a crude ferrous picrate mixture).

[0053] 4) Refining and finished product preparation

[0054] 1. After the reaction is completed, the product 3 in the reactor is filtered through a vacuum filtration device using a Buchner funnel and a suction filtration bottle. The pore size of the filter membrane is selected to be 5-10 microns to remove the unreacted iron powder.

[0055] 2. Detect and analyze the filtered product. Use a moisture meter to detect the moisture content and ensure that it is less than 100ppm; use an atomic absorption spectrometer to detect the iron content and adjust it to 400ppm; use acid-base titration to detect the free picric acid content and control it at 0.4%.

[0056] 3. If the composition of the product does not meet the requirements, it can be fine-tuned by adding an appropriate amount of solvent or other reagents to finally obtain a product 4 (finished product of ferrous picrate fuel additive) that meets the requirements. The solvent is composed of 85% toluene and 15% 2-propanol.

[0057] 4. Product Testing and Analysis

[0058] 1. Infrared spectrum analysis: The final product is tested by infrared spectrum and compared with the infrared spectrum of standard ferrous picrate to confirm whether the structure and composition of the product are correct. -1 There should be a phenolic hydroxyl (OH) peak at 1632-1622cm -1 and 1603-1610cm -1 The aromatic ring vibration peak appears at about 1330cm -1 A strong symmetrical aromatic nitro stretching peak appears at .

[0059] 2. Element analysis: Use atomic absorption spectrometer and other equipment to accurately measure the iron content in the product to verify whether it meets the 400ppm standard. At the same time, other impurity elements are tested to ensure the purity of the product.

[0060] 3. Stability test: Store the product at high temperature (such as 60°C), regularly observe changes in the product's color, transparency and other appearance, detect changes in iron content, free picric acid content and moisture content, and evaluate the product's stability and shelf life. The product should remain stable for a long time without obvious deterioration.

[0061] In summary: In the present invention, by replacing dry picric acid with non-explosive aromatic hydrocarbon / ether picrate, combined with acid treatment of iron powder activation, reasonable selection of solvents (such as mixed aromatic hydrocarbons and lower alcohols) and other means, the safe production of ferrous picrate fuel additives is achieved, and the risk of explosion is effectively avoided. By controlling the moisture content of the reaction system, reacting under anhydrous or low-water conditions, and optimizing the reaction temperature (10-80°C, preferably 30-60°C) and stirring conditions, the function of improving product stability and shelf life is achieved, and it is suitable for high-temperature storage and transportation environments. By controlling the proportion of reaction raw materials (such as the molar ratio of picrate to iron powder), the reaction time (5-15 minutes), and filtering and adjusting the ingredients after the reaction, the function of accurately preparing ferrous picrate fuel additives that meet specific indicators (moisture content less than 100ppm, iron content of 400ppm, free picric acid content of 0.4%, and solvent composed of 85% toluene and 15% 2-propanol) is achieved.

Claims

1. The formula of ferrous picrate fuel additive is characterized by: Prepared by the following steps: Step 1: Prepare solvent mixture: Mix aromatic hydrocarbons and fatty alcohols in a mass ratio of 1:9- 9:1 ​​to obtain an anhydrous or low-water solvent system to obtain product 1; Step 2: Produce ferrous picrate intermediate: add one or both of aromatic hydrocarbon picrate and aromatic ether picrate to the product 1 obtained in step 1, and then add activated iron powder to obtain product 2. The activated iron powder is prepared by washing the iron activated by hydrochloric acid with water and alcohol in turn; Step 3: Synthesis and crude product: in 10- At 80°C, product 2 is allowed to continue to react for a period of time to complete the reaction, thereby obtaining product 3; Step 4: Refining and preparation of finished products: Filter the product 3 obtained in step 3 to remove unreacted iron powder to obtain product 4.

2. The formula of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 1, the aromatic hydrocarbons are one or more of benzene, toluene, xylene, and mixed aromatic hydrocarbons.

3. The formula of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 1, the fatty alcohol is one or more of methanol, ethanol, propanol, butanol, and C5 to C8 alcohols.

4. The formula of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 2, the aromatic hydrocarbon picrate is one or more of benzene picrate, toluene picrate, xylene picrate, and naphthalene picrate.

5. The formula of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 2, the aromatic ether picrate is one or more of anisole picrate and diphenyl ether picrate.

6. The formula of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 2, the acid used in the acid activation treatment is hydrochloric acid, and the treatment time is 30 seconds.

7. The formulation of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 3, the reaction temperature is preferably 30-60°C.

8. The formulation of the ferrous picrate fuel additive as claimed in claim 1, characterized in that: In the step 4, the moisture content of the product 4 is less than 100 ppm, the iron content is 400 ppm, the free picric acid content is 0.4%, and the solvent is composed of 85% toluene and 15% 2-propanol.

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