Method and device for continuously synthesizing spherical micro-nano cuprous oxide powder

A technology of cuprous oxide and powder, which is applied in the field of nanomaterials, can solve problems such as agglomeration, particle shape, uncontrollable size, difficulty in batch consistency control, and insufficient particle size distribution. It achieves easy post-processing, simple structure, Good star effect

Active Publication Date: 2012-09-26
JINCHUAN GROUP LIMITED +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Of course, there are also other documents that have reported the synthesis of spherical cuprous oxide particles, but in these documents a large number of surfactants are used to control the morphology, and the reaction time is longer and the temperature is often higher (by hydrothermal method). )
The particles synthesized by these methods are often agglomerated seriously, and the particle size distribution is not good enough.
Moreover, these methods all adopt the batch production method of tank type crystallization reactor, which cannot be produced continuously, and the consistency control between batches is difficult.
In addition, when using a tank-type crystallization reactor, due to the special growth mechanism of cuprous oxide, the system always explodes repeatedly to generate extremely fine cuprous oxide particles, and once these particles are formed, due to back-mixing, they have already formed In order to reduce the surface energy, the extremely fine particles are adsorbed on the surface of the large particles that stay in the system for a long time, resulting in agglomeration and the shape and size of the particles are completely uncontrollable

Method used

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  • Method and device for continuously synthesizing spherical micro-nano cuprous oxide powder

Examples

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Embodiment 1

[0037] A segmented tubular reaction device (see figure 1 ), which in turn includes a trident pipe, six sections of tubular heating reactors in series and a discharge pipe; between the trifurcated pipe and the tubular heating reactors, and between the tubular heating reactors in series are connected by pipelines; in the first and second Material input pipes are arranged on the pipes between the two-stage tubular heating reactors. The inner diameter of the tube of the tubular reactor is 4mm, and the total length of the tube is 85m. Except for the first section, which is 10m long, the remaining sections are all 15m.

[0038] Process for continuous synthesis of spherical cuprous oxide powder:

[0039](1) Dissolve copper sulfate pentahydrate, sodium hydroxide and glucose in deionized water respectively to prepare 0.2mol / L copper sulfate solution A, 0.55mol / L sodium hydroxide solution B and 0.11mol / L glucose Solution C.

[0040] (2) Put solution A and solution B into the first-st...

Embodiment 2

[0046] The structure of the sectioned tubular reaction device is the same as in Example 1.

[0047] Process for continuous synthesis of spherical cuprous oxide powder:

[0048] (1) Dissolve copper sulfate pentahydrate, sodium hydroxide and glucose in deionized water respectively, and prepare 0.2mol / L copper sulfate solution A, 0.80mol / L sodium hydroxide solution B and 0.11mol / L glucose Solution C.

[0049] (2) Put solution A and solution B into the first-stage tubular reactor at a speed of 20mL / min with advection pump through the trident tube, and control the temperature T of the first-stage tubular reactor 1 at 25°C.

[0050] (3) Add solution C to the reaction system at a rate of 20mL / min through the pipeline between the first and second tubular reactors;

[0051] (4) The mixture system enters the subsequent five-stage tubular reactor at a speed of 60mL / min, and the reaction temperature of each stage is controlled (T 2 , T 3 , T 4 , T 5 , T 6 ) at 40°C, 45°C, 50°C, 55...

Embodiment 3

[0055] The structure of the sectioned tubular reaction device is the same as in Example 1.

[0056] (1) Dissolve copper sulfate pentahydrate, sodium hydroxide and glucose in deionized water respectively, and prepare 0.2mol / L copper sulfate solution A, 0.60mol / L sodium hydroxide solution B and 0.11mol / L glucose Solution C.

[0057] (2) Put solution A and solution B into the first-stage tubular reactor at a speed of 20mL / min with advection pump through the trident tube, and control the temperature T of the first-stage tubular reactor 1 at 30°C.

[0058] (3) Add solution C to the reaction system at a rate of 20mL / min through the pipeline between the first and second tubular reactors;

[0059] (4) The mixture system enters the subsequent five-stage tubular reactor at a speed of 60mL / min, and the reaction temperature of each stage is controlled (T 2 , T 3 , T 4 , T 5 , T 6 ) at 50°C, 55°C, 60°C, 65°C and 70°C, respectively.

[0060] (5) The final product of the reaction col...

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Abstract

The invention provides a method for continuously synthesizing spherical micro-nano cuprous oxide powder, and a segmented pipe type reactor for realizing the method, belonging to the technical field of nanometer materials. The method includes the steps as follows: fully mixing copper sulfate solution with sodium hydroxide solution by a pipeline and then leading the mixed solution to enter the pipetype reactor for preheating; adding glucose solution in the mixed solution; later leading the mixed system to pass through a segment or a serial-connection multi-pipe type reactor so as to raise temperature to 50-70 DEG C in a continuous or gradient way; and filtering the mixed system after oxidation reduction in the pipe type reactor, washing the mixed system with water and ethanol in sequence, conducting vacuum drying, and finally obtaining the spherical micro-nano cuprous oxide powder. The spherical micro-nano cuprous oxide powder obtained by the method is within the range of 0.5-2Mum in particle size and smooth on surface, has a cubic phase in crystal form, and has high uniformity of particle size distribution, excellent dispersivity, good sphericity and high purity. The method is easy to control in synthesizing process, low in cost, energy-saving and environment-friendly, and beneficial to industrialized production.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, and relates to a method for synthesizing spherical micronano cuprous oxide powder, in particular to a method for continuously synthesizing spherical micronano cuprous oxide powder; the present invention also relates to the continuous synthesis of spherical micronano cuprous oxide powder Apparatus for copper powder. Background technique [0002] Cuprous oxide (Cu 2 O) Powder has a wide range of uses in industrial and agricultural production. For example, it is used as a marine primer in the paint industry to prevent marine organisms from adhering; it is used as a fungicide in agriculture; it can be used together with copper as a ballast in the electronics industry. Cuprous oxide ultrafine powder can also be used as photothermal catalyst, smoke suppression and flame retardant material, electrode material, key intermediate material of conductive paste for microelectronic circuit printing, in...

Claims

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Application Information

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IPC IPC(8): C01G3/02B82Y40/00
Inventor 吴有庭杨志强王栋白志平武浚唐乐吕晓华刘会基朱用贺建军
Owner JINCHUAN GROUP LIMITED
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