CN1302884C - Method and apparatus for preparing mixed powder of nano gold and sodium chloride - Google Patents

Method and apparatus for preparing mixed powder of nano gold and sodium chloride Download PDF

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Publication number
CN1302884C
CN1302884C CNB2004100892560A CN200410089256A CN1302884C CN 1302884 C CN1302884 C CN 1302884C CN B2004100892560 A CNB2004100892560 A CN B2004100892560A CN 200410089256 A CN200410089256 A CN 200410089256A CN 1302884 C CN1302884 C CN 1302884C
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sodium chloride
gold
mixed powder
heater
powder
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CN1663716A (en
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黄德欢
李宗全
吕春菊
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SHANGHAI HUASHI NANO MATERIAL CO Ltd
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Abstract

The present invention discloses a method for preparing mixed nanometer-gold and sodium chloride powder, which comprises: (1) a chloroauric acid water solution with the mass percentage concentration of 0.2 to 5.0% is prepared by deionized water; (2) sodium chloride is added to the chloroauric acid water solution, and the mass ratio of the chloroauric acid to the sodium chloride is from 1:1 to 1:100; after the sodium chloride is completely dissolved, the solution is dried at the temperature of 50 to 95 DEG C, then milled and crushed; (3) the powder obtained in step (2) is put in a heater, argon or air is led into the heater, the powder is heated at the temperature of 250 to 450 DEG C for 0.2 to 3 hours, and the furnace temperature is reduced to the room temperature as the argon or air is continuously led into the heater. The present invention has the advantages of simple technology and low cost; the present invention is friendly to the environment, and does not discharge toxic or harmful substances to the outside. The prepared products only contain nanometer gold and sodium chloride without materials such as dispersing agents, surfactants, etc., and therefore, is safe to eat.

Description

The method and the device that prepare nm of gold sodium chloride mixed powder
Technical field
The present invention relates to a kind of method and device for preparing nm of gold sodium chloride mixed powder.
Background technology
Claim gold that the effect of " town's spirit, hard marrow, tonneau the five internal organs perverse trend, the angle of clothes " is arranged in the Compendium of Material Medica that Li Shizhen (1518-1593 A.D.) is write.Nm of gold has a wide range of applications at numerous areas such as medical treatment, health care, biochemical industries, thereby is paid much attention to.At present, nm of gold with the reducing process preparation, has often been added in preparation disadvantageous dispersant of human body and surfactant mostly, has influence on the use of nm of gold.
Summary of the invention
The object of the present invention is to provide a kind of method and device for preparing nm of gold sodium chloride mixed powder safe to eat.
The method for preparing nm of gold sodium chloride mixed powder of the present invention, its step is as follows:
1) with deionized water preparation mass percent concentration is 0.2~5.0% gold chloride (HAuCl 44H 2O) aqueous solution;
2) sodium chloride is joined in the aqueous solution of chloraurate, the mass ratio of gold chloride and sodium chloride is 1: 1~1: 100, treats sodium chloride all after the dissolving, with solution 50~95 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into heater, feeds argon gas or air, and gas flow is 1~10 liter/minute, after heating 0.2 to 3 hour under 250~450 ℃, in continuing ventilation, reduce furnace temperature,, obtain nm of gold and sodium chloride mixed powder until room temperature.
The device for preparing nm of gold sodium chloride mixed powder with the inventive method, comprise body of heater, place the reactor in the body of heater, reactor is made of quartz ampoule and ceramic boat, ceramic boat is positioned at quartz ampoule, one end of quartz ampoule has air inlet, and the other end is provided with blast pipe, and blast pipe is connected successively with the container of containing sodium hydrate aqueous solution and the container that is filled with water.Utilize sodium hydrate aqueous solution and water to absorb gold chloride and decompose chlorine and the hydrogen chloride that is discharged.
The present invention utilizes gold chloride (HAuCl 44H 2O) stability not high, at a lower temperature with regard to decomposable characteristics, the mixture of gold chloride and sodium chloride is heated under proper temperature, acquisition is dispersed in the nm of gold in the sodium chloride, make nm of gold keep its polymolecularity, the gold content of nm of gold is 0.5~32% in the mixed powder, the granularity of nm of gold is 20nm to 150nm, and is safe to eat.Preparation technology of the present invention is simple, and cost is low, in the product that makes, only contains nm of gold and sodium chloride, does not contain other materials such as dispersant, surfactant.Environmentally friendly, the external discharging of no poisonous, harmful substance.
Description of drawings
Fig. 1 is the device schematic diagram of preparation nm of gold sodium chloride mixed powder;
Fig. 2 is the X-ray diffractogram of embodiment 1 nm of gold and sodium chloride mixed powder, and gold content is 2.5%, and the particle mean size of gold is 56nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride;
Fig. 3 is the X-ray diffractogram of embodiment 2 nm of gold and sodium chloride mixed powder, and gold content is 2.5%, and the particle mean size of gold is 90nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride;
Fig. 4 is the X-ray diffractogram of embodiment 3 nm of gold and sodium chloride mixed powder, and gold content is 10.0%, and the particle mean size of gold is 95nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride;
Fig. 5 is the X-ray diffractogram of embodiment 4 nm of gold and sodium chloride mixed powder, and gold content is 20.0%, and the particle mean size of gold is 134nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride.
The specific embodiment
With reference to Fig. 1, the device of preparation nano gold powder, comprise body of heater 1, place the reactor in the body of heater, reactor is made of quartz ampoule 2 and ceramic boat 3, and ceramic boat 3 is positioned at quartz ampoule 2, and an end of quartz ampoule has air inlet 4, the other end is provided with blast pipe 5, and blast pipe is connected successively with the container 6 of containing sodium hydrate aqueous solution and the container 7 that is filled with water.Utilize sodium hydrate aqueous solution and water to absorb gold chloride and decompose chlorine and the hydrogen chloride that is discharged.
Embodiment 1
1) with deionized water preparation mass percent concentration is 1.0% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 4.7g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 70 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feeds argon gas, and argon flow amount is 1 liter/minute, after heating 1 hour under 250 ℃, in continuing ventilation, reduce furnace temperature,, obtain the nm of gold of gold content 2.5% and the mixed powder of sodium chloride until room temperature.
Fig. 2 is the nm of gold that makes and the X-ray diffractogram of sodium chloride mixed powder, and the particle mean size of gold is 56nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride.
Embodiment 2
1) with deionized water preparation mass percent concentration is 1.0% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 4.7g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 80 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feeds argon gas, and argon flow amount is 1 liter/minute, after heating 2 hours under 300 ℃, in continuing ventilation, reduce furnace temperature,, obtain the nm of gold of gold content 2.5% and the mixed powder of sodium chloride until room temperature.
Fig. 3 is the X-ray diffractogram of nm of gold and sodium chloride mixed powder, and the particle mean size of gold is 90nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride.
Embodiment 3
1) with deionized water preparation mass percent concentration is 4.0% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 4.3g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 85 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feeds argon gas, and argon flow amount is 5 liters/minute, after heating 1 hour under 350 ℃, in continuing ventilation, reduce furnace temperature,, obtain the nm of gold of gold content 10.0% and the mixed powder of sodium chloride until room temperature.
Fig. 4 is the X-ray diffractogram of nm of gold and sodium chloride mixed powder, and the particle mean size of gold is 95nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride.
Embodiment 4
1) with deionized water preparation mass percent concentration is 4.0% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 4.3g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 85 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feeds argon gas, and argon flow amount is 5 liters/minute, after heating 20 minutes under 400 ℃, in continuing ventilation, reduce furnace temperature,, obtain the nm of gold of gold content 10.0% and the mixed powder of sodium chloride until room temperature.
Fig. 5 is the X-ray diffractogram of nm of gold and sodium chloride mixed powder, and the particle mean size of gold is 134nm, and " * " number marked golden diffraction maximum among the figure, and remaining diffraction maximum is a sodium chloride.
Embodiment 5
1) with deionized water preparation mass percent concentration is 4.0% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 1.0g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 85 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feed argon gas, argon flow amount is 5 liters/minute, after heating 0.5 hour under 300 ℃, in continuing ventilation, reduce furnace temperature, until room temperature, obtain the nm of gold of gold content 32.4% and the mixed powder of sodium chloride, the particle mean size of gold is 140nm.
Embodiment 6
1) with deionized water preparation mass percent concentration is 0.5% gold chloride (HAuCl 44H 2O) aqueous solution 25ml;
2) 5.0g sodium chloride is joined in the aqueous solution of chloraurate, treat that sodium chloride is all after the dissolving, 90 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into the ceramic boat of heater, feed argon gas, argon flow amount is 1 liter/minute, after heating 0.5 hour under 250 ℃, in continuing ventilation, reduce furnace temperature, until room temperature, obtain the nm of gold of gold content 1.2% and the mixed powder of sodium chloride, the particle mean size of gold is 44nm.

Claims (1)

1. the method for preparing nm of gold sodium chloride mixed powder is characterized in that step is as follows:
1) with deionized water preparation mass percent concentration is 0.2~5.0% aqueous solution of chloraurate;
2) sodium chloride is joined in the aqueous solution of chloraurate, the mass ratio of gold chloride and sodium chloride is 1: 1~1: 100, treats sodium chloride all after the dissolving, with solution 50~95 ℃ of oven dry down, then with its grinding, pulverizing;
3) with step 2) powder that obtains puts into heater, feeds argon gas or air, and gas flow is 1~10 liter/minute, after heating 0.2 to 3 hour under 250~450 ℃, in continuing ventilation, reduce furnace temperature,, obtain nm of gold and sodium chloride mixed powder until room temperature.
CNB2004100892560A 2004-12-02 2004-12-02 Method and apparatus for preparing mixed powder of nano gold and sodium chloride Expired - Fee Related CN1302884C (en)

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CN1302884C true CN1302884C (en) 2007-03-07

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05339298A (en) * 1992-06-05 1993-12-21 Taiyo Kagaku Co Ltd Production of protein-polysaccharide complex compound
JPH06136488A (en) * 1992-04-09 1994-05-17 Nippon Steel Corp Ferritic stainless steel excellent in workability, high temperature salt damage resistance, and high temperature strength
US5427634A (en) * 1992-04-09 1995-06-27 Nippon Steel Corporation Ferrite system stainless steel having excellent nacl-induced hot corrosion resistance and high temperature strength
CN1240689A (en) * 1998-07-08 2000-01-12 中国科学技术大学 Process for preparing superfine powder by thermolyzing metal complex
CN1241638A (en) * 1998-07-09 2000-01-19 浙江大学 Smelting method and equipment for nanometer hard tungsten-cobalt carbide alloy

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06136488A (en) * 1992-04-09 1994-05-17 Nippon Steel Corp Ferritic stainless steel excellent in workability, high temperature salt damage resistance, and high temperature strength
US5427634A (en) * 1992-04-09 1995-06-27 Nippon Steel Corporation Ferrite system stainless steel having excellent nacl-induced hot corrosion resistance and high temperature strength
JPH05339298A (en) * 1992-06-05 1993-12-21 Taiyo Kagaku Co Ltd Production of protein-polysaccharide complex compound
CN1240689A (en) * 1998-07-08 2000-01-12 中国科学技术大学 Process for preparing superfine powder by thermolyzing metal complex
CN1241638A (en) * 1998-07-09 2000-01-19 浙江大学 Smelting method and equipment for nanometer hard tungsten-cobalt carbide alloy

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