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Solvent thermal constant-pressure synthesis method for controlling phase of carbon nitride material

A synthesis method and carbon nitride technology, applied in the fields of nitrogen and non-metallic compounds, nitrogen purification/separation, etc., can solve the problems of difficult preparation conditions, reduce the application value of products, damage the selectivity of the reaction process, etc., and achieve high application value. , to achieve the effect of low-cost large-scale synthesis and scale-up of preparation

Inactive Publication Date: 2008-09-03
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have their own limitations: for example, in addition to controlling the reaction temperature, it is almost impossible for us to control other influencing factors in the reactor, so it is difficult to quickly optimize the preparation conditions to achieve low yield of the two materials. cost mass synthesis
In addition, when the reaction process is completed and the temperature begins to drop, the original cubic structure phase may also undergo phase reversal, causing multiple phases to coexist in the product, which seriously damages the selectivity of the reaction process and reduces the application value of the product.

Method used

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  • Solvent thermal constant-pressure synthesis method for controlling phase of carbon nitride material
  • Solvent thermal constant-pressure synthesis method for controlling phase of carbon nitride material
  • Solvent thermal constant-pressure synthesis method for controlling phase of carbon nitride material

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Example 1: firstly add metal sodium flakes into benzene, and distill after standing for 24 hours to remove water and oxygen therein. Then under the protection of nitrogen, weigh the stoichiometric ratio of sodium azide (NaN 3 ) and trichloroazine (C 3 N 3 Cl 3 ) into the autoclave, then add 8ml of dried benzene and then seal it. Apply a pressure of 40 MPa on the autoclave, then control the temperature of the autoclave to rise to 220 °C at a rate of 0.01 °C / min, react at constant temperature and pressure for 8 hours, and then naturally cool to room temperature.

[0039] After the reaction, the benzene was first filtered off with suction, and then the product was washed with acetone, ethanol, and dilute hydrochloric acid in sequence to remove organic by-products and other impurities, and then the product was repeatedly washed with deionized water until the filtrate was neutral. Heating the product in vacuum to 60°C for drying can obtain graphite carbon nitride (g-C 3...

Embodiment 2

[0040] Example 2: As described in Example 1, the difference is that the reaction temperature is increased to 260°C.

Embodiment 3

[0041] Embodiment 3: As described in Embodiment 1, the difference is that the reaction temperature of the autoclave is increased to 300° C., trichloroazine is replaced by trimethylamine, and sodium azide is replaced by nitrogen trichloride.

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Abstract

A method for controlling the phase of carbon nitride material by solvent heating constant pressure synthesis belongs to fields of chemical production and new material. The method includes preparing carbon source solution and nitrogen source solution; feeding into a reaction kettle; applying constant pressure of 40-2,000MPa before heating; heating up to 220-1,000 DEG C at a heating rate of 0.01-60 DEG C / min; cooling after the reaction is completed; and post-treating the product. When the boron carbon nitride is synthesized by the method, temperature and pressure of the reaction system can be independently controlled, so that the reaction can be carried out under the constant pressure, and the pressure of the reaction system can be varied according to the requirement so as to control the speed and the direction of the reaction for synthesizing boron carbon nitride. The method is capable of preparing high-particle size carbon nitride crystal.

Description

[0001] This application is 200610042101.0, a divisional application titled "A Solvothermal Constant Pressure Synthesis Method for Regulating the Phase of Boron Carbon Nitride Material", with an application date of January 4, 2006. 1. Technical field [0002] The invention relates to a solvothermal constant-pressure synthesis method for regulating the phase of boron-carbon-nitrogen materials, which belongs to the field of new chemical materials. 2. Background technology [0003] As superhard materials with excellent performance, cubic boron nitride, diamond, and carbon nitride (collectively referred to as boron carbon nitride) have played and will soon play a pivotal role in daily life and industrial production. The artificial synthesis of these materials, especially Low-cost mass synthesis has always been the dream of human beings. In order to realize this ideal, various preparation methods have been developed and improved, among which the high temperature and high pressure ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/082C01B21/04C01B31/06C01B31/04
Inventor 崔得良陆希峰赖泽锋朱玲玲王琪珑蒋民华
Owner SHANDONG UNIV
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