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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 directions 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 mass synthesis and scale-up of preparation

Inactive Publication Date: 2010-02-10
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: First, metal sodium flakes were added to benzene, and after standing for 24 hours, it was distilled to remove water and oxygen. Then under the protection of nitrogen, weigh out the stoichiometric ratio of sodium azide (NaN 3 ) And trichloroazine (C 3 N 3 Cl 3 ) Put it into the autoclave, add 8ml of dried benzene and seal it. A pressure of 40 MPa was applied to the autoclave, and the temperature of the autoclave was controlled to rise to 220° C. at a rate of 0.01° C. / min, and the temperature and pressure was reacted for 8 hours and then naturally cooled to room temperature.

[0039] After the reaction, the benzene is firstly filtered off with suction, and then the product is washed successively with acetone, ethanol, and dilute hydrochloric acid to remove organic by-products and other impurities, and then the product is washed repeatedly with deionized water until the filtrate is neutral. Heating the product in vacuum to 60°C for drying, then graphite carbon nitr...

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] Example 3: As described in Example 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 0.01-60DEG 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 a divisional application of 200610042101.0, titled "A solvothermal constant pressure synthesis method for regulating and controlling the phase of boron carbon nitrogen material", and the application date was January 4, 2006. 1. Technical Field [0002] The invention relates to a solvothermal constant pressure synthesis method for regulating and controlling the phase of boron carbon nitrogen materials, and belongs to the field of new chemical materials. 2. Background technology [0003] Cubic boron nitride, diamond, and carbon nitride (collectively referred to as boron carbon nitride) are super-hard materials with excellent performance. They have and will play a pivotal role in daily life and industrial production to realize the artificial synthesis of these materials, especially Low-cost mass synthesis has always been a dream of mankind. In order to realize this ideal, people have developed and improved various preparation methods, among which the high t...

Claims

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Application Information

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Patent Type & Authority Patents(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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