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A kind of organic sulfide rare earth metal layered compound and preparation method thereof

A technology for sulfiding rare earth compounds, applied in organic chemistry and other fields, can solve problems such as poor compatibility and restrictions on the application and development of rare earth metal compounds, and achieve the effects of improved dispersibility, simple preparation method, and environmentally friendly preparation process

Active Publication Date: 2018-02-06
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, rare earth materials, as inorganic materials, have poor compatibility with rubber materials, which restricts the application and development of rare earth metal compounds in rubber.

Method used

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  • A kind of organic sulfide rare earth metal layered compound and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Weigh 5.1g MgCl 2 ·6H 2 O and 4.1g La(NO 3 ) 3 ·6H 2 O, dissolved in 100mL to remove CO 2 Mg in ionized water 2 + / La 3+ Aqueous solution; weigh 0.4g NaOH and 2.1g NaNO 3 , add 100mL to CO 2 Ionized water is made into alkaline solution;

[0041] A 500mL three-necked flask with a stirring device and a thermometer is used as a reaction vessel, and the above alkali solution is poured into it, and the Mg 2+ / La 3+ The aqueous solution was added dropwise to the alkali solution at 10.0mL / min, and the reaction temperature was controlled at 20°C;

[0042] Mg 2+ / La 3+ After the aqueous solution is added dropwise, add 4.0g of bis(γ-triethoxypropyl) disulfide and 0.4g of polyethylene glycol, heat up to 60°C, stir the solution at 60°C for 2h, filter, wash, After drying, the organic lanthanum sulfide layered compound MgLa-LDHs is obtained, and its molecular formula is

[0043] [Mg 2+ 0.67 La 3+ 0.33 (OH) 2 ] 0.33+ (NO 3 - ) 0.33 ·[S-(CH 2 ) 3 -Si(OH) 3 ] ...

Embodiment 2

[0045] Weigh 5.1g MgCl 2 ·6H 2 O and 4.1g La(NO 3 ) 3 ·6H 2 O, dissolved in 100mL to remove CO 2 Mg in ionized water 2 + / La 3+ Aqueous solution; weigh 0.4g NaOH and 2.1g NaNO 3 , add 100mL to CO 2 Ionized water is made into alkaline solution;

[0046] A 500mL three-necked flask with a stirring device and a thermometer is used as a reaction vessel, and the above alkali solution is poured into it, and the Mg 2+ / La 3+ The aqueous solution was added dropwise to the alkali solution at 3.0mL / min, and the reaction temperature was controlled at 50°C;

[0047] Mg 2+ / La 3+ After the aqueous solution is added dropwise, add 7.3g of bis(γ-triethoxypropyl)tetrasulfide, 0.4g of hexanethiol and 0.6g of polyethylene glycol, heat to raise the reaction temperature, and keep the solution at 90°C for stirring reaction After 0.5h, after cooling to room temperature, filter, wash, and dry to obtain the organic lanthanum sulfide layered compound MgLa-LDHs, whose molecular formula is ...

Embodiment 3

[0050] Weigh 18.3g MgCl 2 ·6H 2 O and 11.5g Y(NO 3 ) 3 ·6H 2 O, dissolved in 100mL to remove CO 2 Mg in ionized water 2+ / Y 3+ Aqueous solution; weigh 1.0g NaOH and 0.9g NaNO 3 , add 100mL to CO 2 Ionized water is made into alkaline solution;

[0051] A 500mL three-necked flask with a stirring device and a thermometer is used as a reaction vessel, and the above alkali solution is poured into it, and the Mg 2+ / Y 3+ The aqueous solution was added dropwise to the alkali solution at 5.0mL / min, and the reaction temperature was controlled at 50°C;

[0052] Mg 2+ / Y 3+ After the aqueous solution has been added dropwise, add 9.5g of bis(γ-triethoxypropyl) disulfide, 3.3g of 2-mercaptophenylprophiazole and 0.8g of polyethylene glycol, and heat the temperature of the reaction solution to 85°C. The solution was stirred and reacted at 85°C for 1 hour, cooled to room temperature after the reaction, filtered, washed and dried to obtain the organic yttrium sulfide layered compo...

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Abstract

The present invention proposes an organosulfide rare earth metal layered compound, the trivalent metal ion of the layered compound layer plate is a rare earth metal ion, and the compound structure also contains an organic sulfur group, and the alkyl group in the structure can improve the compound and macromolecule The compatibility of polymers can also inhibit the agglomeration between layered compounds. The present invention also provides a preparation method of the compound, which adopts the co-precipitation method, adds an organic sulfur-containing compound in the preparation process of the layered compound, and prepares an organosulfide rare earth metal layered compound by one-step reaction. The process is simple, the raw materials are easy to obtain, and the energy Low consumption and good repeatability.

Description

technical field [0001] The invention belongs to the field of organic compounds, in particular to a layered compound containing organic groups and rare earth metals and a preparation method of the layered compound. Background technique [0002] There are a large number of empty orbitals in the atomic structure of rare earth elements, the electronic energy levels are extremely rich, and the chemical properties are active. Adding them to rubber can show their unique effects. The development and utilization of rare earth metal compounds as additives in the field of rubber industry has become a hot spot of extensive research. . Due to the special atomic structure of rare earth elements, the physical and chemical properties of rare earth rubber additives in rubber formulations are superior to those of traditional rubber additives, and their application and development prospects are very broad. Chinese patent CN1219553A reports that a rare earth rubber vulcanization accelerator ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F19/00C08K3/30C08J3/24C08L21/00
Inventor 赵丽丽董栋刘哲
Owner BEIJING RED AVENUE INNOVA