Preparation method and application of diethyl aluminum hypophosphite

Abstract

The invention provides a preparation method and application of diethyl aluminum hypophosphite, and the preparation method comprises the following steps: (1) adding sodium hypophosphite monohydrate, water-insoluble organic acid and an initiator into a reaction kettle, replacing and exhausting air in the reaction kettle with nitrogen, introducing ethylene gas into the reaction kettle, and reacting to obtain diethylaluminum hypophosphite; a diethyl hypophosphorous acid solution is obtained; (2) extracting and layering the diethyl hypophosphorous acid solution with water, wherein an obtained water layer is a diethyl hypophosphorous acid aqueous solution; (3) reacting the diethyl hypophosphorous acid aqueous solution with aluminum sulfate, and filtering after the reaction is finished to obtain a diethyl aluminum hypophosphite crude product; and washing and drying the crude product to obtain the diethyl aluminum hypophosphite. The initiator used in the invention has high purity, and the synthetic method has high product yield and high purity. According to the method, the diethyl hypophosphorous acid is extracted from the water-insoluble organic acid by using water, and the recycled organic acid can be reused, so that the environmental protection pressure is reduced, and the energy consumption is reduced.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of preparation, and particularly relates to a preparation method and application of aluminum diethylphosphinate. BACKGROUND

[0002] Aluminum diethylphosphinate is a compound with a molecular formula of Al(PO2C4H10)3, a CAS number of 225789-38-8 and a molar mass of 390.3 g / mol, and is a member of the family of organophosphinates. The compound has a white powder appearance, good fluidity and a density of 1.35 g / cm3.

[0003] Aluminum diethylphosphinate is used as an excellent halogen-free flame retardant for engineering plastics such as polyamides, polyesters, thermosets and elastomers. In UL94 flammability tests, glow wire ignition temperature (GWIT) and glow wire flammability index (GWFI) tests and tracking index (CTI), aluminum diethylphosphinate exhibits excellent performance in glass fiber reinforced polyamide 6 and 66 composites and various polyesters (PBT and PET). Aluminum diethylphosphinate can not only play a role in the condensed phase to promote polymer carbonization, but also remove high-energy radicals in the combustion zone. Aluminum diethylphosphinate is often used in combination with other halogen-free flame retardants or synergists (such as melamine polyphosphate and melamine cyanurate).

[0004] Aluminum diethylphosphinate has the characteristics of environmental and health friendliness, and is used as an excellent halogen-free flame retardant for engineering plastics such as polyamides, polyesters, thermosets and elastomers; aluminum diethylphosphinate can not only play a role in the condensed phase to promote polymer carbonization, but also remove high-energy radicals in the combustion zone; aluminum diethylphosphinate has the characteristics of environmental and health friendliness.

[0005] At present, the synthesis method of diethylphosphinate mainly adopts a free radical addition method, that is, an olefin reacts with hypophosphorous acid under the action of an initiator to generate a dialkyl hypophosphite. A large amount of acetic acid is used in these methods, and after the reaction is completed, the acetic acid needs to be removed. The recovered acetic acid needs to be treated before being recycled, which has high energy consumption and great environmental pressure. SUMMARY

[0006] The purpose of the present application is to provide a preparation method and application of aluminum diethylphosphinate.

[0007] In order to achieve the above purpose, the present application provides the following technical solutions. A preparation method of aluminum diethylphosphinate, the preparation method comprising the following steps: (1) adding sodium hypophosphite monohydrate, water-insoluble organic acid and initiator into a reaction kettle, replacing the air in the reaction kettle with nitrogen, and then charging ethylene gas into the reaction kettle to react, thereby obtaining a diethyl hypophosphite solution; (2) extracting the diethyl hypophosphite solution with water to separate the layers, and the obtained water layer is a diethyl hypophosphite aqueous solution; (3) reacting the diethyl hypophosphite aqueous solution with aluminum sulfate, filtering after the reaction is completed, thereby obtaining a diethyl aluminum hypophosphite crude product; and washing and drying the obtained crude product, thereby obtaining diethyl aluminum hypophosphite.

[0008] Further, the water-insoluble organic acid is at least one of hexanoic acid, heptanoic acid and nonanoic acid.

[0009] Further, the water-insoluble organic acid is a mixture of hexanoic acid, heptanoic acid and nonanoic acid at a mass ratio of 1:1.2-1.5:0.4-0.7.

[0010] Further, the feeding amount of the water-insoluble organic acid is 1-3 times the mass of the sodium hypophosphite monohydrate.

[0011] Further, the initiator is di-tert-butyl peroxide.

[0012] Further, the mass of the initiator is 2-3% of the mass of the sodium hypophosphite monohydrate.

[0013] Further, the preparation method of di-tert-butyl peroxide is as follows: (1) first, adding tert-butyl alcohol with a mass percentage concentration of 85% into a first reaction container, and adding sulfuric acid with a mass percentage concentration of 85% into the tert-butyl alcohol in the first reaction container in a dropwise manner under stirring and at a temperature of 30°C, and controlling the reaction time to be 160-180 min, thereby obtaining a tert-butyl hydrogen sulfate esterification liquid, and the molar ratio of the tert-butyl alcohol to the sulfuric acid is 1:0.35-0.39; while stirring, controlling the stirring temperature to be 10-12°C, and slowly adding hydrogen peroxide with a mass percentage concentration of 30-40% into a second reaction container to which a reused mother liquor is added, and reacting for 60-80 min, thereby obtaining a mixed liquid, and the weight ratio of the hydrogen peroxide to the reused mother liquor is 1:2.5-3; while stirring, controlling the reaction temperature to be 8-12°C, and slowly adding the tert-butyl hydrogen sulfate esterification liquid into a third reaction container to which the mixed liquid is added, and the weight ratio of the tert-butyl hydrogen sulfate esterification liquid to the mixed liquid is 1:3.2-3.5, and the reaction time is 200-250 min, thereby obtaining a reaction product; introducing the reaction product into a liquid separation device to separate the liquid, thereby obtaining an upper oil phase which is a crude tert-butyl hydroperoxide product, and the crude product is a mixture containing hydrogen peroxide and di-tert-butyl peroxide; and performing alkali washing on the crude tert-butyl hydroperoxide product to obtain a di-tert-butyl peroxide crude product; (2) the di-tert-butyl peroxide crude product in step (1) is washed with a washing liquid to obtain a di-tert-butyl peroxide intermediate crude product; (3) the di-tert-butyl peroxide intermediate crude product in step (2) is washed with alkali, washed with water, and dried to obtain a di-tert-butyl peroxide finished product.

[0014] Further, the mass ratio of the washing liquid to the di-tert-butyl peroxide crude product is 1:2-3.

[0015] Further, the washing temperature is 20-30℃, and the washing time is 30-60min. Further, the washing liquid is a tert-butyl alcohol sulfate esterification liquid; and the preparation steps are as follows: mixing sulfuric acid and tert-butyl alcohol, and reacting at 20-30℃ for 15-30min; wherein the mass fraction of sulfuric acid after mixing is 30-50wt%, and the mass fraction of tert-butyl alcohol is 30-50wt%.

[0016] Further, in the alkali washing, the mass ratio of the alkali washing liquid to the di-tert-butyl peroxide crude product is: di-tert-butyl peroxide crude product: alkali washing liquid = 1:1-1.2.

[0017] Further, in step (1), the reaction temperature is 100-120℃, the reaction time is 8-10h, and the ethylene pressure during the reaction is 0.3-0.8MPa.

[0018] Further, in step (3), the reaction temperature is 90-95℃, and the reaction time is 3-4h.

[0019] An application of a preparation method of diethyl aluminum hypophosphite.

[0020] Compared with the prior art, the application has the following advantages and beneficial effects: 1. The product yield of the synthesis method is high, and the purity is high. In the application, diethyl hypophosphite is extracted from the organic acid which is insoluble in water by using water, the recovered organic acid can be reused, the cost is greatly saved, the process is simplified, the environmental pressure is reduced, and the energy consumption is reduced, compared with other methods.

[0021] 2. The purity of di-tert-butyl peroxide as an initiator has a direct impact on the yield and purity of the reaction. High-purity initiators can reduce side reactions caused by impurities, ensuring that more initiator molecules can effectively decompose into free radicals to initiate polymerization. Impurities may react undesirably with monomers or other reaction components, resulting in the formation of unexpected byproducts, thereby reducing yield. High-purity initiators make reaction conditions easier to control, which helps maintain a constant initiation rate, thereby obtaining more consistent and predictable products. If the initiator contains impurities, these impurities may affect the initiator's decomposition rate, leading to changes in the polymerization rate and, in turn, affecting the molecular weight distribution of the final product. Using high-purity initiators can reduce the impurity content in the reaction system and help improve the purity of the final product. The presence of impurities may cause the appearance of unwanted components in the product, affecting product performance. High-purity initiators help produce purer products. DETAILED DESCRIPTION

[0022] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0023] Example 1 This embodiment provides a method for preparing diethyl aluminum hypophosphite, which comprises the following steps: (1) Sodium hypophosphite monohydrate, a water-insoluble organic acid, and an initiator are added to a reactor. After the air in the reactor is completely replaced with nitrogen, ethylene gas is introduced into the reactor to react to obtain a diethyl hypophosphite solution; (2) The diethyl hypophosphorous acid solution is extracted with water and the resulting aqueous layer is the diethyl hypophosphorous acid aqueous solution; (3) The aqueous solution of diethyl hypophosphite is reacted with aluminum sulfate, and after the reaction is completed, the solution is filtered to obtain a crude product of diethyl hypophosphite aluminum; the crude product is washed with water and dried to obtain diethyl hypophosphite aluminum.

[0024] The water-insoluble organic acid is at least one of hexanoic acid, heptanoic acid, and nonanoic acid.

[0025] The water-insoluble organic acid is a mixture of hexanoic acid, heptanoic acid and nonanoic acid in a mass ratio of 1:1.2:0.7.

[0026] The mass of the water-insoluble organic acid is twice the mass of the sodium hypophosphite monohydrate.

[0027] The initiator is di-tert-butyl peroxide.

[0028] The mass of the initiator is 2.5% of the mass of sodium hypophosphite monohydrate.

[0029] The preparation method of di-tert-butyl peroxide is as follows: (1) First, tert-butyl alcohol with a mass percentage concentration of 85% is added to a first reaction container, and under stirring and with the temperature controlled at 30℃, sulfuric acid with a mass percentage concentration of 85% is added dropwise into the tert-butyl alcohol in the first reaction container to react, and the reaction time is controlled at 170 min, to obtain a tert-butyl hydrogen sulfate esterification liquid, and the molar ratio of the tert-butyl alcohol to the sulfuric acid is 1:0.36; while stirring, the stirring temperature is controlled at 11℃, and hydrogen peroxide with a mass percentage concentration of 35% is slowly added into a second reaction container with a reused mother liquor to react for 70 min, to obtain a mixed liquid, and the weight ratio of the hydrogen peroxide to the reused mother liquor is 1:2.8; while stirring, the reaction temperature is controlled at 10℃, and the tert-butyl hydrogen sulfate esterification liquid is slowly added into a third reaction container with the mixed liquid, and the weight ratio of the tert-butyl hydrogen sulfate esterification liquid to the mixed liquid is 1:3.4, and the reaction time is 220 min, to obtain a reaction product; the reaction product is introduced into a liquid separation device to separate, to obtain an upper oil phase as a crude tert-butyl hydroperoxide, which is a mixture containing hydrogen peroxide and di-tert-butyl peroxide; the crude tert-butyl hydroperoxide is subjected to alkali washing to obtain a crude di-tert-butyl peroxide; (2) The crude di-tert-butyl peroxide in step (1) is washed with a washing liquid to obtain an intermediate crude di-tert-butyl peroxide; (3) The intermediate crude di-tert-butyl peroxide in step (2) is subjected to alkali washing, water washing, and drying to obtain a finished di-tert-butyl peroxide.

[0030] The mass ratio of the washing liquid to the crude di-tert-butyl peroxide is 1:2.5.

[0031] The washing temperature is 25℃, and the washing time is 40 min. The washing liquid is a tert-butyl alcohol sulfate esterification liquid; and the preparation steps are as follows: mixing sulfuric acid and tert-butyl alcohol, and reacting at 25℃ for 20 min; wherein, after mixing, the mass percentage of the sulfuric acid is 40 wt%, and the mass percentage of the tert-butyl alcohol is 60 wt%.

[0032] In the alkali washing, the mass ratio of the alkali washing liquid to the crude di-tert-butyl peroxide is: crude di-tert-butyl peroxide: alkali washing liquid = 1:1.1.

[0033] In step (1), the reaction temperature is 110℃, the reaction time is 9 h, and the ethylene pressure during the reaction is 0.5 MPa.

[0034] In step (3), the reaction temperature is 92℃, and the reaction time is 3.5 h.

[0035] Example 2 The embodiment provides a preparation method of aluminum diethyl hypophosphite. (1) adding sodium hypophosphite monohydrate, water-insoluble organic acid and initiator into a reaction kettle, replacing air in the reaction kettle with nitrogen, and then filling ethylene gas into the reaction kettle to react, so as to obtain a diethyl hypophosphite solution; (2) the diethyl hypophosphite solution is extracted with water to separate into layers, and the obtained water layer is diethyl hypophosphite aqueous solution; (3) the diethyl hypophosphite aqueous solution is reacted with aluminum sulfate, and after the reaction is completed, filtration is performed to obtain crude aluminum diethyl hypophosphite; and after the obtained crude product is washed with water and dried, aluminum diethyl hypophosphite is obtained.

[0036] The water-insoluble organic acid is at least one of hexanoic acid, heptanoic acid and nonanoic acid.

[0037] The water-insoluble organic acid is a mixture of hexanoic acid, heptanoic acid and nonanoic acid with a mass ratio of 1:1.2:0.4.

[0038] The feeding mass of the water-insoluble organic acid is 1 times the mass of the sodium hypophosphite monohydrate.

[0039] The initiator is di-tert-butyl peroxide.

[0040] The mass of the initiator is 2% of the mass of the sodium hypophosphite monohydrate.

[0041] The preparation method of the di-tert-butyl peroxide is as follows: (1) first, tert-butyl alcohol with a mass percentage concentration of 85% is added into a first reaction container, and tert-butyl hydroperoxide esterification liquid is obtained by adding mass percentage concentration of 85% sulfuric acid into the tert-butyl alcohol in the first reaction container in a dropwise manner under stirring and temperature control of 30 ℃, and the molar ratio of the tert-butyl alcohol to the sulfuric acid is 1:0.35; while stirring, hydrogen peroxide with a mass percentage concentration of 30% is slowly added into a second reaction container to which a reused mother liquor is added, and a mixed liquid is obtained after 60 min of reaction, wherein the weight ratio of the hydrogen peroxide to the reused mother liquor is 1:2.5; while stirring, the reaction temperature is controlled to be 8 ℃, and the tert-butyl hydroperoxide esterification liquid is slowly added into a third reaction container to which the mixed liquid is added, and the weight ratio of the tert-butyl hydroperoxide esterification liquid to the mixed liquid is 1:3.2, and the reaction time is 200 min, so as to obtain a reaction product; the reaction product is introduced into a liquid separation device for liquid separation, and the upper oil phase is a crude tert-butyl hydroperoxide product, which is a mixture containing hydrogen peroxide and di-tert-butyl peroxide; the crude tert-butyl hydroperoxide product is subjected to alkali washing to obtain a di-tert-butyl peroxide crude product; (2) washing the crude di-tert-butyl peroxide of step (1) with a washing liquid to obtain an intermediate crude di-tert-butyl peroxide; (3) obtaining a finished di-tert-butyl peroxide by washing, water washing and drying the intermediate crude di-tert-butyl peroxide of step (2).

[0042] The mass ratio of the washing liquid to the crude di-tert-butyl peroxide is 1:2.

[0043] The washing temperature is 20℃ and the washing time is 30 min. The washing liquid is a tert-butyl alcohol esterification liquid of sulfuric acid; the preparation steps are: mixing sulfuric acid and tert-butyl alcohol at 20℃ for 15 min; wherein the mass fraction of sulfuric acid after mixing is 30% and the mass fraction of tert-butyl alcohol is 70%.

[0044] The mass ratio of the washing liquid to the crude di-tert-butyl peroxide is 1:2.

[0045] In step (1), the reaction temperature is 100℃, the reaction time is 8h, and the ethylene pressure during the reaction is 0.3MPa.

[0046] In step (3), the reaction temperature is 90℃ and the reaction time is 3h.

[0047] Example 3 The present embodiment provides a preparation method of aluminum diethyl hypophosphite, which comprises the following steps: (1) adding sodium hypophosphite monohydrate, water-insoluble organic acid and initiator into a reaction kettle, replacing the air in the reaction kettle with nitrogen, and then filling ethylene gas into the reaction kettle to react, to obtain a diethyl hypophosphite solution; (2) extracting and separating the diethyl hypophosphite solution with water, and the obtained water layer is a diethyl hypophosphite aqueous solution; (3) reacting the diethyl hypophosphite aqueous solution with aluminum sulfate, filtering after the reaction, to obtain a crude aluminum diethyl hypophosphite; and drying the obtained crude product to obtain aluminum diethyl hypophosphite.

[0048] The water-insoluble organic acid is at least one of hexanoic acid, heptanoic acid and nonanoic acid.

[0049] The water-insoluble organic acid is a mixture of hexanoic acid, heptanoic acid and nonanoic acid with a mass ratio of 1:1.2:0.7.

[0050] The feeding mass of the water-insoluble organic acid is 3 times the mass of sodium hypophosphite monohydrate.

[0051] The initiator is di-tert-butyl peroxide.

[0052] The mass of the initiator is 3% of the mass of sodium hypophosphite monohydrate.

[0053] The preparation method of di-tert-butyl peroxide is as follows: (1) First, tert-butyl alcohol with a mass percentage concentration of 85% is added to a first reaction container, and under stirring and with the temperature controlled at 30℃, sulfuric acid with a mass percentage concentration of 85% is added dropwise into the tert-butyl alcohol in the first reaction container for reaction, and the reaction time is controlled at 180 min, to obtain a tert-butyl hydrogensulfate esterification liquid, and the molar ratio of the tert-butyl alcohol to the sulfuric acid is 1:0.39; while stirring, the stirring temperature is controlled at 12℃, and hydrogen peroxide with a mass percentage concentration of 40% is slowly added into a second reaction container added with a recycled mother liquor for reaction for 80 min, to obtain a mixed liquid, wherein the weight ratio of the hydrogen peroxide to the recycled mother liquor is 1:3; while stirring, the reaction temperature is controlled at 12℃, and the tert-butyl hydrogensulfate esterification liquid is slowly added into a third reaction container added with the mixed liquid, and the weight ratio of the tert-butyl hydrogensulfate esterification liquid to the mixed liquid is 1:3.5, and the reaction time is 250 min, to obtain a reaction product; the reaction product is introduced into a liquid separation device for liquid separation, to obtain an upper oil phase which is a crude tert-butyl hydroperoxide, and the crude product is a mixture containing hydrogen peroxide and di-tert-butyl peroxide; the crude tert-butyl hydroperoxide is subjected to alkali washing to obtain a crude di-tert-butyl peroxide; (2) The crude di-tert-butyl peroxide in step (1) is washed with a washing liquid to obtain an intermediate crude di-tert-butyl peroxide; (3) The intermediate crude di-tert-butyl peroxide in step (2) is subjected to alkali washing, water washing, and drying to obtain a finished di-tert-butyl peroxide.

[0054] The mass ratio of the washing liquid to the crude di-tert-butyl peroxide is 1:3.

[0055] The washing temperature is 30℃, and the washing time is 60 min. The washing liquid is a tert-butyl alcohol sulfate esterification liquid; and the preparation steps are as follows: mixing sulfuric acid and tert-butyl alcohol, and reacting at 30℃ for 30 min; wherein the mass percentage of the sulfuric acid after mixing is 50 wt%, and the mass percentage of the tert-butyl alcohol after mixing is 50 wt%.

[0056] The mass ratio of the alkali washing liquid to the crude di-tert-butyl peroxide is: crude di-tert-butyl peroxide: alkali washing liquid = 1:1.2.

[0057] In step (1), the reaction temperature is 120℃, the reaction time is 10 h, and the ethylene pressure during the reaction is 0.8 MPa.

[0058] In step (3), the reaction temperature is 95℃, and the reaction time is 4 h.

[0059] Comparative Example 1 The difference between the present comparative example and Example 1 is that the initiator is di-tert-butyl peroxide; the mass of the initiator is 1.5% of the mass of sodium hypophosphite monohydrate.

[0060] Comparative Example 2 The difference between the present comparative example and Example 1 is that the washing liquid is a tert-butyl alcohol esterification liquid of sulfuric acid; the preparation procedure is that sulfuric acid and tert-butyl alcohol are mixed, and the mixture is reacted at 20℃ for 10 min; wherein, after mixing, the mass fraction of sulfuric acid is 20%, and the mass fraction of tert-butyl alcohol is 80%.

[0061] Comparative Example 3 The difference between the present comparative example and Example 1 is that in step (1), the reaction temperature is 80℃, the reaction time is 6 h, and the ethylene pressure during the reaction is 0.2 Pa.

[0062] Performance Test The products prepared in the examples and comparative examples are subjected to performance test, and the results are shown in Table 1.

[0063] Table 1: Performance test results

[0064] From the above performance test results, it can be seen that the yield and purity of Examples 1-3 are high, and the comprehensive performance of Example 1 is the most outstanding. The comparative examples are obviously poorer than the examples in the corresponding performance tests because they do not use the necessary technical solutions. The above experimental results further prove the importance of the technical solutions defined in the present application to the technical effects.

[0065] The above is the preferred embodiment of the present application. It should be noted that for ordinary skilled persons in the technical field, some improvements and refinements can be made without departing from the principles of the present application, and these improvements and refinements should also be considered as the protection scope of the present application.

Claims

1. A method for preparing diethyl aluminum hypophosphite, characterized in that: The preparation method comprises the following steps: (1) Sodium hypophosphite monohydrate, a water-insoluble organic acid, and an initiator are added to a reactor. After the air in the reactor is completely replaced with nitrogen, ethylene gas is introduced into the reactor to react to obtain a diethyl hypophosphite solution; (2) The diethyl hypophosphorous acid solution is extracted with water and the resulting aqueous layer is the diethyl hypophosphorous acid aqueous solution; (3) The aqueous solution of diethyl hypophosphite is reacted with aluminum sulfate, and after the reaction is completed, the solution is filtered to obtain a crude product of diethyl hypophosphite aluminum; the crude product is washed with water and dried to obtain diethyl hypophosphite aluminum.

2. The method for preparing diethyl aluminum hypophosphite according to claim 1, wherein The initiator is di-tert-butyl peroxide; the mass of the initiator is 2-3% of the mass of sodium hypophosphite monohydrate.

3. The method for preparing diethyl aluminum hypophosphite according to claim 1, wherein The preparation method of di-tert-butyl peroxide is: (1) First, tert-butyl alcohol with a mass percentage concentration of 85% is added to a first reaction container, and sulfuric acid with a mass percentage concentration of 85% is added dropwise to the tert-butyl alcohol in the first reaction container under stirring and at a temperature of 30° C. to react, and the reaction time is controlled to be 160-180 minutes to obtain tert-butyl hydrogen sulfate esterification liquid, wherein the molar ratio of the tert-butyl alcohol to the sulfuric acid is 1:0.35-0.39; while stirring and controlling the stirring temperature to be 10-12° C., hydrogen peroxide with a mass percentage concentration of 30-40% is slowly added dropwise to a second reaction container to which the recycled mother liquor is added, and the reaction is carried out for 60-80 minutes to obtain a mixture. The method comprises the following steps: preparing a mixture of the hydrogen peroxide and the recycled mother liquor in a weight ratio of 1:2.5-3; controlling the reaction temperature at 8-12° C. while stirring; slowly adding the tert-butyl hydrogen sulfate esterification liquid dropwise to a third reaction vessel containing the mixed liquid, wherein the weight ratio of the tert-butyl hydrogen sulfate esterification liquid to the mixed liquid is 1:3.2-3.5; and reacting for 200-250 minutes to obtain a reaction product; introducing the reaction product into a liquid separator for separation to obtain an upper oil phase of crude tert-butyl hydroperoxide, which is a mixture containing hydrogen peroxide and di-tert-butyl peroxide; and alkali washing the crude tert-butyl hydroperoxide to obtain crude di-tert-butyl peroxide. (2) washing the crude di-tert-butyl peroxide product of step (1) with a washing solution to obtain an intermediate crude di-tert-butyl peroxide product; (3) The intermediate crude product of di-tert-butyl peroxide in step (2) is subjected to alkali washing, water washing, and drying to obtain a finished product of di-tert-butyl peroxide.

4. The method for preparing diethyl aluminum hypophosphite according to claim 3, wherein: The mass ratio of the washing liquid to the crude di-tert-butyl peroxide is 1:2-3.

5. The method for preparing diethyl aluminum hypophosphite according to claim 3, wherein: The washing liquid is tert-butyl sulfate esterification liquid; The preparation steps are as follows: mixing sulfuric acid and tert-butanol, and reacting them at 20-30° C. for 15-30 minutes; wherein the sulfuric acid and tert-butanol are 30-50 wt% and 30-50 wt% respectively after mixing.

6. The method for preparing diethyl aluminum hypophosphite according to claim 3, wherein: The washing mass ratio of the alkaline washing liquid to the crude di-tert-butyl peroxide in the alkaline washing is: crude di-tert-butyl peroxide: alkaline washing liquid = 1:1-1.

2.

7. The method for preparing diethyl aluminum hypophosphite according to claim 1, wherein: The mass of the water-insoluble organic acid is 1-3 times the mass of the sodium hypophosphite monohydrate.

8. The method for preparing diethyl aluminum hypophosphite according to claim 1, wherein: In step (1), the reaction temperature is 100-120°C, the reaction time is 8-10 hours, and the ethylene pressure during the reaction is 0.3-0.8 MPa.

9. The method for preparing diethyl aluminum hypophosphite according to claim 1, wherein: In step (3), the reaction temperature is 90-95°C and the reaction time is 3-4h.

10. Use of the method for preparing diethylaluminum hypophosphite according to any one of claims 1 to 9.

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