A rare earth modified talc powder compound, a preparation method and application thereof

Abstract

The application discloses a rare earth modified talc powder compound and a preparation method and application thereof, which is prepared from cerium citrate, boric acid and talc powder through continuous two-stage calcination in an air atmosphere, wherein the mass ratio of the cerium citrate, the boric acid and the talc powder is 20-80:20-80:2-5, in the two-stage calcination, the temperature of the first-stage calcination is 250-400 DEG C, the time of the first-stage calcination is 1-3h, the temperature of the second-stage calcination is 700-1000 DEG C, and the time of the second-stage calcination is 1-3h. The rare earth modified talc powder compound is prepared by using a sintering method, is used as a functional modification additive of a ternary ethylene-propylene-diene rubber, can improve electrolyte resistance and mechanical properties of the ternary ethylene-propylene-diene rubber, and thus improves the service life of the ternary ethylene-propylene-diene rubber into a negative pressure suction nozzle.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of rare earth functional materials, and particularly relates to a rare earth modified talc powder compound and a preparation method and application thereof. BACKGROUND

[0002] In the production process of lithium ion batteries, the formation process of the battery is the initial activation process of the battery and the first charging process. In this process, the battery will undergo an electrochemical reaction, and a passivation layer will be formed at the interface of the carbon negative electrode and the electrolyte. At the same time, a large amount of gas will be generated. If the gas accumulates in the battery, it will cause irreversible damage to the battery. Therefore, a rubber formation negative pressure suction nozzle is needed to vacuum the gas accumulated in the battery, which requires the rubber to have the characteristics of resisting multiple extrusion stretching and resisting electrolyte corrosion. The ethylene-propylene-diene rubber has a high cost performance and is often used as a formation negative pressure suction nozzle material. In order to further improve the tensile strength, elongation at break and electrolyte corrosion resistance of the ethylene-propylene-diene rubber, the heat-resistant electrolyte corrosion resistance and mechanical properties of the ethylene-propylene-diene rubber need to be modified. SUMMARY

[0003] The application aims to overcome the defects of the prior art and provide a rare earth modified talc powder compound.

[0004] Another object of the application is to provide a preparation method of the rare earth modified talc powder compound.

[0005] Still another object of the application is to provide an application of the rare earth modified talc powder compound.

[0006] The technical scheme of the application is as follows:

[0007] A rare earth modified talc powder compound is prepared by continuous two-stage calcination of cerium citrate, boric acid and talc powder in an air atmosphere, wherein the mass ratio of cerium citrate, boric acid and talc powder is 20-80:20-80:2-5, the temperature of the first-stage calcination is 250-400 DEG C, the time of the first-stage calcination is 1-3h, the temperature of the second-stage calcination is 700-1000 DEG C, and the time of the second-stage calcination is 1-3h.

[0008] The preparation method of the rare earth modified talc powder compound comprises the following steps:

[0009] (1) mixing cerium nitrate, citric acid and deionized water to react to obtain cerium citrate;

[0010] (2) the cerium citrate, boric acid and talc powder obtained in step (1) are blended uniformly, and then two-stage calcination is carried out in an air atmosphere, wherein the first-stage calcination is carried out at a temperature of 250-400 DEG C for 1-3 h, and the second-stage calcination is carried out at a temperature of 700-1000 DEG C for 1-3 h.

[0011] In a preferred embodiment of the present application, in step (1), the molar ratio of citric acid to cerium nitrate is 1-6:1.

[0012] Use of the above rare earth modified talc powder compound in the preparation of functional ethylene propylene diene rubber.

[0013] In a preferred embodiment of the present application, the functional ethylene propylene diene rubber is prepared by mixing and vulcanizing ethylene propylene diene rubber (EPDM), sulfur (S), 2-mercaptobenzothiazole (DPTT), sulfur donor DPTT, carbon black and the rare earth modified talc powder compound (CeO2@Talc) of claim 1.

[0014] Further preferably, the mass ratio of the ethylene propylene diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the above rare earth modified talc powder compound is 100:0.5-3.0:0.8-2.5:0.4-1.0:20-50:10-60.

[0015] A functional ethylene propylene diene rubber, which raw materials include the above rare earth modified talc powder compound.

[0016] In a preferred embodiment of the present application, the functional ethylene propylene diene rubber is prepared by mixing and vulcanizing ethylene propylene diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the above rare earth modified talc powder compound.

[0017] Further preferably, the mass ratio of the ethylene propylene diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the above rare earth modified talc powder compound is 100:0.5-3.0:0.8-2.5:0.4-1.0:20-50:10-60.

[0018] The present application has the following advantages:

[0019] 1. The rare earth modified talc powder compound of the present application is prepared by sintering, and is used as a functional modification aid for ethylene propylene diene rubber, which can improve the electrolyte resistance and mechanical properties of the ethylene propylene diene rubber, thereby improving the service life of the ethylene propylene diene rubber formed into a negative pressure suction nozzle.

[0020] 2、The rare earth modified talc compound has good corrosion resistance compared with pure talc powder, and can improve the electrolyte resistance of EPDM. BRIEF DESCRIPTION OF DRAWINGS

[0021] Figure 1 The scanning electron microscope photo of the rare earth modified talc compound prepared in Example 1. DETAILED DESCRIPTION

[0022] The technical solutions of the present application are further described and explained in detail through specific embodiments combined with the drawings.

[0023] Example 1

[0024] (1) 1 mol of cerium nitrate, 3 mol of citric acid and 100 mol of deionized water were placed in a three-necked flask and reacted at 30℃ for 3h, ammonia water was added to adjust the pH value to 6, and a precipitate was obtained; the precipitate was filtered out and washed with alcohol for 3-5 times, and then placed in a vacuum oven and dried at 100℃ for 7h to obtain cerium citrate.

[0025] (2) 50 parts by weight of cerium citrate, 50 parts by weight of talc and 3 parts by weight of boric acid were uniformly blended and placed in a muffle furnace, first calcined at 400℃ for 2h, and then heated to 700℃ for further calcination for 3h to obtain a cerium oxide@talc (CeO2@Talc) compound as shown in Figure 1 .

[0026] Example 2

[0027] (1) 1 mol of cerium nitrate, 6 mol of citric acid and 150 mol of deionized water were placed in a three-necked flask and reacted at 30℃ for 3h, ammonia water was added to adjust the pH value to 6, and a precipitate was obtained; the precipitate was filtered out and washed with deionized water for 3-5 times, and then placed in a vacuum oven and dried at 100℃ for 8h to obtain cerium citrate;

[0028] (2) 20 parts by weight of cerium citrate, 80 parts by weight of talc and 5 parts by weight of boric acid were uniformly blended and placed in a muffle furnace, first calcined at 250℃ for 3h, and then heated to 800℃ for further calcination for 3h to obtain a cerium oxide@talc (CeO2@Talc) compound.

[0029] Example 3

[0030] (1) Put 1 mol of cerium nitrate, 4 mol of citric acid and 120 mol of deionized water into a three-necked flask, react at 30°C for 3 h, add ammonia water to adjust the pH value to 6 to obtain a precipitate; filter out the precipitate and wash the filter with deionized water for 3-5 times, and then place it in a vacuum oven, dry at 100°C for 7 h to obtain cerium citrate;

[0031] (2) Put 80 parts by weight of cerium citrate, 20 parts by weight of talc powder and 2 parts by weight of boric acid into a muffle furnace, first calcine at 350°C for 2 h, then continue to calcine at 1000°C for 2 h to obtain the cerium oxide@talc (CeO2@Talc) compound.

[0032] Example 4

[0033] (1) Put 1 mol of cerium nitrate, 4 mol of citric acid and 120 mol of deionized water into a three-necked flask, react at 30°C for 3 h, add ammonia water to adjust the pH value to 6 to obtain a precipitate; filter out the precipitate and wash the filter with deionized water for 3-5 times, and then place it in a vacuum oven, dry at 100°C for 7 h to obtain cerium citrate;

[0034] (2) Put 80 parts by weight of cerium citrate, 20 parts by weight of talc powder and 2 parts by weight of boric acid into a muffle furnace, first calcine at 350°C for 2 h, then continue to calcine at 1000°C for 2 h to obtain the cerium oxide@talc (CeO2@Talc) compound.

[0035] Example 5

[0036] (1) Put 100 parts by weight of EPDM at 85°C into a double roller open mill and plasticize uniformly;

[0037] (2) First, uniformly premix 2 parts by weight of S, 1 part by weight of accelerator M, 0.5 parts by weight of DPTT, 50 parts by weight of carbon black and 20 parts by weight of CeO2@Talc prepared in Example 1, then slowly add them into the open mill, fully mix for 3 min to obtain a sheet-shaped rubber compound;

[0038] (3) After the rubber compound is placed for 24 h, vulcanize it on a vulcanizing machine at 150°C for 6 min to obtain a rare earth modified EPDM.

[0039] Example 6

[0040] (1) Put 100 parts by weight of EPDM at 85°C into a double roller open mill and plasticize uniformly;

[0041] (2) 0.5 parts by weight of S, 2 parts by weight of accelerator M, 1 part by weight of DPTT, 30 parts by weight of carbon black and 50 parts by weight of CeO2@Talc prepared in Example 1 were uniformly premixed, and then slowly added into an open mill, and fully mixed for 3 min to obtain a sheet-like mixed rubber;

[0042] (3) After the mixed rubber was placed for 24 h, it was vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a rare earth modified EPDM.

[0043] Example 7

[0044] (1) 100 parts by weight of EPDM was uniformly plasticized on a two-roll open mill at 85°C;

[0045] (2) 3 parts by weight of S, 0.8 parts by weight of accelerator M, 0.4 parts by weight of DPTT, 50 parts by weight of carbon black and 10 parts by weight of CeO2@Talc prepared in Example 1 were uniformly premixed, and then slowly added into an open mill, and fully mixed for 3 min to obtain a sheet-like mixed rubber;

[0046] (3) After the mixed rubber was placed for 12 h, it was vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a rare earth modified EPDM.

[0047] Example 8

[0048] (1) 100 parts by weight of EPDM was uniformly plasticized on a two-roll open mill at 85°C;

[0049] (2) 1 part by weight of S, 1.5 parts by weight of accelerator M, 1 part by weight of DPTT, 20 parts by weight of carbon black and 60 parts by weight of CeO2@Talc prepared in Example 1 were uniformly premixed, and then slowly added into an open mill, and fully mixed for 3 min to obtain a sheet-like mixed rubber;

[0050] (3) After the mixed rubber was placed for 18 h, it was vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a rare earth modified EPDM.

[0051] Example 9

[0052] (1) 100 parts by weight of EPDM was uniformly plasticized on a two-roll open mill at 85°C;

[0053] (2) 2 parts by weight of S, 1 part by weight of accelerator M, 1 part by weight of DPTT, 40 parts by weight of carbon black and 40 parts by weight of CeO2@Talc prepared in Example 1 were uniformly premixed, and then slowly added into an open mill, and fully mixed for 3 min to obtain a sheet-like mixed rubber;

[0054] (3) After the mixed rubber was placed for 24 h, it was vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a rare earth modified EPDM.

[0055] Comparative Example 1

[0056] (1) 100 parts by weight of EPDM was placed on a two-roll open mill after constant temperature at 85°C and plasticized uniformly;

[0057] (2) 2 parts by weight of S, 1 part by weight of accelerator M, 1 part by weight of DPTT, and 40 parts by weight of carbon black were pre-mixed uniformly and then slowly added to the open mill, and fully mixed for 3 min to obtain a sheet-shaped mixed rubber;

[0058] (3) The mixed rubber was placed for 24 h, and then vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a comparative modified EPDM.

[0059] Comparative Example 2

[0060] (1) 100 parts by weight of EPDM was placed on a two-roll open mill after constant temperature at 85°C and plasticized for 3 min;

[0061] (2) 2 parts by weight of S, 1 part by weight of accelerator M, 1 part by weight of DPTT, 40 parts by weight of carbon black, and 40 parts by weight of talc were pre-mixed uniformly and then slowly added to the open mill, and fully mixed for 3 min to obtain a sheet-shaped mixed rubber;

[0062] (3) The mixed rubber was placed for 24 h, and then vulcanized on a vulcanizing machine at 150°C for 6 min to obtain a comparative modified EPDM.

[0063] The performance comparison of Examples 5-9 and Comparative Examples 1-2 is as follows:

[0064]

[0065] From Examples 5 to 9, it can be seen that after adding CeO2@Talc in EPDM, the tensile strength and elongation at break of EPDM can be simultaneously improved, and the volume change rate after immersion in electrolyte is also low.

[0066] The above description is only a preferred embodiment of the present application, and therefore cannot limit the scope of the present application. Any equivalent changes and modifications made according to the scope of the present patent and the content of the specification shall still be within the scope of the present application.

Claims

1. A rare earth modified talc powder compound characterized by: The rare earth modified talc powder compound is prepared by two-stage calcination in air atmosphere from cerium citrate, boric acid and talc powder, wherein the mass ratio of cerium citrate, boric acid and talc powder is 20-80:20-80:2-5, and the temperature of the first stage calcination is 250-400℃, the time of the first stage calcination is 1-3h, the temperature of the second stage calcination is 700-1000℃, and the time of the second stage calcination is 1-3h.

2. A process for the preparation of a rare earth modified talc powder compound as claimed in claim 1, characterized in that: The method comprises the following steps: (1) mixing cerium nitrate, citric acid and deionized water to obtain cerium citrate; (2) blending the cerium citrate obtained in step (1), boric acid and talc powder uniformly, and then performing two-stage calcination in air atmosphere, wherein the temperature of the first stage calcination is 250-400℃, the time of the first stage calcination is 1-3h, the temperature of the second stage calcination is 700-1000℃, and the time of the second stage calcination is 1-3h.

3. The production method according to claim 2, characterized by: In step (1), the molar ratio of citric acid to cerium nitrate is 1-6:

1.

4. Use of the rare earth modified talc powder compound of claim 1 in the preparation of functional ethylene-propylene-diene rubber.

5. The use according to claim 4, wherein: The functional ethylene-propylene-diene rubber is prepared by mixing and vulcanizing ethylene-propylene-diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the rare earth modified talc powder compound of claim 1.

6. The use according to claim 5, characterized in that: The mass ratio of the ethylene-propylene-diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the rare earth modified talc powder compound of claim 1 is 100:0.5-3.0:0.8-2.5:0.4-1.0:20-50:10-60.

7. A functional ethylene propylene diene rubber characterized by: The raw materials thereof comprise the rare earth modified talc powder compound of claim 1.

8. A functional EPDM rubber according to claim 7, characterized in that: The functional ethylene-propylene-diene rubber is prepared by mixing and vulcanizing ethylene-propylene-diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the rare earth modified talc powder compound of claim 1.

9. A functional EPDM rubber as claimed in claim 8, characterized in that: The mass ratio of the ethylene-propylene-diene rubber, sulfur, 2-mercaptobenzothiazole, sulfur donor DPTT, carbon black and the rare earth modified talc powder compound of claim 1 is 100:0.5-3.0:0.8-2.5:0.4-1.0:20-50:10-60.

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