1275571 九、發明說明： 【發明所屬之技術領域】 本發明係-種製備奈米金溶液的方法，特別是_種以氯金酸曰人 ΐίϊϊϊΓ水溶祕室訂糊^料奈料驗龄法。心 奈米金在醫療、保健、生物化卫等諸多領域有廣泛的庫用價值， 高度重視。奈米金具有空氣淨化功能，可用作奈米金觸 奈米金溶液可喷塗在各觀料表面，如金屬、轉、喊和1275571 IX. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a method for preparing a nanogold solution, in particular, a chlorinated acid 曰 ϊϊϊΓ ϊϊϊΓ ϊϊϊΓ ϊϊϊΓ ϊϊϊΓ 订 订 订 订 订 。 。 。 。 。 。 。 。 。 。. Heart Nano Kim has extensive library value in many fields such as medical care, health care, and biochemistry, and attaches great importance to it. Nano-gold has an air purification function and can be used as a nano-gold nano-gold solution that can be sprayed on various surfaces such as metal, turn, shout and
採用的還原法製備奈米金溶液需要在攝氏7叱或更高 【發明内容】 本發明的目的在於提供-種在室溫下製備奈米金溶液的方法 發明的製備奈米金溶液的方法，其步驟如下·· (1)在去離子水巾加人氯金酸（ΗΑυα4·4Η2())，待氯金酸溶解後加 入聚乙烯财_、十二絲硫酸鈉形成混合溶液，氣金酸、聚乙稀 轉細和十二絲硫咖的f量濃度分職讀〜1G%、⑽2〜2〇% 和 0.0001〜1.0% ; ' 0 (2)至/皿下’在授拌中將濃度A 〇 〇1〜〇 5%的水合肼水溶液加入到步 驟⑴的混合溶液中’當pH值達到6.8〜7.0時，停止加入水合肼水溶液， 繼續攪拌20〜30分鐘，得到奈米金溶液。 本發明的優點是：製備在室溫下進行，製程簡單，奈米金溶液中 奈米金的粒度為10至100 nm，金粒子小，不易發生沉殿。 【實施方式】 實施例一之步驟為： (1) 將o.lg(克)氣金酸（HAuC14.4H20)加入到250ml(毫升)去離子 水中，待氣金酸溶解後加入〇_2g聚乙烯吡咯烷酮和〇.〇〇〇lg十二院基 硫酸鈉形成混合溶液； (2) 室溫下，在攪拌中將濃度為〇 〇5%的水合肼水溶液加入到步驟⑴ 1275571 的混合溶液中，當pH值達到7 G時，停止加人水 掉^鐘，得到含金量為嶋％的奈米金溶液。 、，k、4 請參閱圖—所示，為依上述本發明實施例-製得的奈米金溶液在 • 攝^如㈣乾後拍攝的x射線衍射圖，H-巾只有金的衍射峰，圖一 中記號標出了金的衍射峰，金粒子的平均直径為丨5肺(夺 實施例二之步驟為： 斤⑴將O.lg氣金酸（HAuClr4H2〇)加入到250ml去離子水中，待 氯金酸溶解後加入aig聚乙烯,比洛細和〇 lg十二絲硫酸納混 合溶液； Φ 、（2)室溫下，在攪拌中將濃度為0趟的水合肼水溶液加入到步驟⑴ 的此口 /合液中’當PH值達到7.0時，停止加入水合肼水溶液，繼續攪 拌20分鐘’得到含金量為0.019%的奈米金溶液。 凊再配合圖二所示，為依上述實施例二製得的奈米金的電子顯微 像圖’金粒子的平均直徑為18nm，圖二中右上角插圖為金粒子的電子 衍射圖。 請再配合圖三所示，是上述實施例二製得之奈米金溶液在攝氏％ C烘乾後拍攝的X射線衍射圖，由金、氣化鈉和少量硫酸肼組成，圖 二中* β己號標出了金的衍射峰，金粒子的平均直徑為，圖三中未 Φ 標出的衍射峰為硫酸肼。 實施例三之步驟為： (1) 將0.3g氣金酸（HAuC14.4H20)加入到50ml去離子水中，待氯 金酸溶解後加入0.2g聚乙烯吡咯烷酮、〇.ig十二烷基硫酸鈉形成混合 溶液； ’ (2) 室溫下’在攪拌中將濃度為〇·2%的水合肼水溶液加入到步驟Q) 的混合溶液中，當pH值達到7.0時，停止加入水合肼水溶液，繼續攪 拌_25分鐘，得到含金量為〇·29%的奈米金溶液，金粒子的平均直徑為 22 nm ° 實施例四之步驟為： 1275571 ⑴將0.06g氣金酸（HAuCl4.4H20)加入到250ml去離子水中，待 氯金酸溶解後加入〇.〇lg聚乙烯吡咯烷酮、〇.〇oolg十二烷基硫酸鈉形 成混合溶液； (2)室溫下，在攪拌中將濃度為0.1%的水合肼水溶液加入到步驟(1) '的混合溶液中，當pH值達到7.0時，停止加入水合肼水溶液，繼續攪 拌20分鐘’得到含金量為〇 〇1%的奈米金溶液，金粒子的平均直徑為 17 nm ° 實施例五之步驟為： ⑴將〇.6g氯金酸（HAuClr4H2〇)加入到50ml去離子水中，待氣 _ 金酸溶解後加入聚乙烯吡咯烷酮、〇.5g十二烷基硫酸鈉形成混合 溶液； (2)室溫下，在攪拌中將濃度為〇·05%的水合肼水溶液加入到步驟(1) 的to合/谷液中，當pH值達到7.0時，停止加入水合肼水溶液，繼續撥 拌30分鐘，得到含金量為〇·57%的奈米金溶液，金粒子的平均直徑為 21 nm ° 實施例六之步驟為： ⑴將〇.8g氯金酸（HAuC14_4H2〇)加入到50ml去離子水中，待氣 金酸溶解後加入l.Og聚乙烯吡咯烷酮、〇.6g十二烷基硫酸鈉形成混合 溶液， (2)室溫下，在攪拌中將濃度為〇·15%的水合肼水溶液加入到步驟 的混合溶液中，當pH值達到7.0時，停止加入水合肼水溶液，繼續攪 拌30分4里’得到含金量為0.76%的奈米金溶液，金粒子的平均直徑為 25 nm ° 【圖式簡單說明】 圖一為室溫下製備的奈米金溶液在攝氏8〇°c烘乾後拍攝的χ射線 衍射圖； '、、 圖二為室溫下製備的奈米金的電子顯微像圖； 圖三為室溫下製備的奈米金溶液在攝氏85°c烘乾後拍攝的χ射線 1275571 衍射圖。 【主要元件符號說明】The method for preparing a nano gold solution by the reduction method needs to be 7 Å or higher. SUMMARY OF THE INVENTION The object of the present invention is to provide a method for preparing a nano gold solution by preparing a nano gold solution at room temperature. The steps are as follows: (1) Adding chloroauric acid (ΗΑυα4·4Η2()) to the deionized water towel, after the chloroauric acid is dissolved, adding polyethylene _, sodium dodecyl sulfate to form a mixed solution, gas gold acid , the amount of concentration of polystyrene and fine sulphur coffee is divided into 1G%, (10) 2~2〇% and 0.0001~1.0%; ' 0 (2) to / under the dish 'concentration in the mixing A 〇〇1~〇5% hydrazine hydrate aqueous solution is added to the mixed solution of the step (1). When the pH value reaches 6.8 to 7.0, the addition of the hydrazine hydrate aqueous solution is stopped, and stirring is continued for 20 to 30 minutes to obtain a nano gold solution. The invention has the advantages that the preparation is carried out at room temperature, and the process is simple. The nano gold in the nano gold solution has a particle size of 10 to 100 nm, and the gold particles are small, and the sinking is not easy to occur. [Examples] The steps of the first embodiment are as follows: (1) Adding o.lg (gram) of gas gold acid (HAuC 14.4H20) to 250 ml (ml) of deionized water, and adding 〇_2g to the gas after the dissolution of the gas gold acid a mixture solution of vinylpyrrolidone and 〇.〇〇〇lg 12-sodium sulfate; (2) adding 5% aqueous hydrazine hydrate solution to the mixed solution of step (1) 1275571 at room temperature, When the pH reached 7 G, the addition of human water was stopped to obtain a nano gold solution containing 嶋% of gold. , k, 4, as shown in the figure - is the x-ray diffraction pattern of the nano gold solution prepared according to the above embodiment of the present invention after the film is dried, and the H-ray has only the diffraction peak of gold. The symbol in Figure 1 indicates the diffraction peak of gold. The average diameter of the gold particles is 丨5 lung (the steps of the second embodiment are: jin (1) adding O.lg gas gold acid (HAuClr4H2 〇) to 250 ml of deionized water. After the chloroauric acid is dissolved, aig polyethylene, a mixture solution of blister and 〇l 12 silk sulphate is added; Φ, (2) at room temperature, a solution of hydrazine hydrate having a concentration of 0 加入 is added to the step of stirring. (1) In this mouth/liquid mixture, when the pH value reaches 7.0, stop adding hydrazine hydrate aqueous solution and continue stirring for 20 minutes to obtain a nano gold solution containing 0.019% gold. The electron micrograph of nano gold prepared in Example 2 has an average diameter of 18 nm. The upper right corner of Figure 2 is an electron diffraction pattern of gold particles. Please refer to Figure 3 above for the second embodiment. The X-ray diffraction pattern of the prepared nano gold solution after drying at 5% C, , gasification of sodium and a small amount of barium sulfate composition, in Figure 2, *β has been marked with a gold diffraction peak, the average diameter of the gold particles is, the diffraction peak marked in Figure 3 is not Φ is barium sulfate. The steps are as follows: (1) adding 0.3 g of gaseous gold acid (HAuC 14.4H20) to 50 ml of deionized water, and after dissolving the chloroauric acid, adding 0.2 g of polyvinylpyrrolidone and 〇.ig sodium dodecyl sulfate to form a mixed solution; ' (2) Add a concentration of 水·2% hydrazine hydrate solution to the mixed solution of step Q) at room temperature. When the pH reaches 7.0, stop adding hydrazine hydrate solution and continue stirring for _25 minutes. A nano gold solution having a gold content of 〇·29% is obtained, and the average diameter of the gold particles is 22 nm °. The procedure of the fourth embodiment is: 1275571 (1) 0.06 g of gas gold acid (HAuCl 4.4H20) is added to 250 ml of deionized water. After the chloroauric acid is dissolved, 〇.〇lg polyvinylpyrrolidone, 〇.〇oolg sodium lauryl sulfate is added to form a mixed solution; (2) a 0.1% aqueous solution of hydrazine hydrate is added to the mixture at room temperature under stirring. Step (1) 'In the mixed solution, when the pH reaches 7.0, stop adding The aqueous solution of hydrazine was added and stirring was continued for 20 minutes to obtain a nanogold solution having a gold content of 〇〇1%. The average diameter of the gold particles was 17 nm. The procedure of Example 5 was as follows: (1) 〇.6g of chloroauric acid (HAuClr4H2〇) Adding to 50ml of deionized water, after the dissolution of gold_goldic acid, adding polyvinylpyrrolidone, 〇5g of sodium lauryl sulfate to form a mixed solution; (2) at room temperature, the concentration is 〇·05% under stirring The aqueous solution of hydrazine hydrate is added to the to/valley solution of step (1). When the pH reaches 7.0, the addition of the aqueous solution of hydrazine hydrate is stopped, and mixing is continued for 30 minutes to obtain a nano gold solution containing 〇·57% of gold. The average diameter of the gold particles is 21 nm °. The steps of the sixth embodiment are as follows: (1) 〇.8g of chloroauric acid (HAuC14_4H2〇) is added to 50ml of deionized water, and after the dissolution of the gas gold acid, 1.0g of polyvinylpyrrolidone is added. .6g sodium lauryl sulfate to form a mixed solution, (2) adding a concentration of 〇15% hydrazine hydrate aqueous solution to the mixed solution of the step under stirring at room temperature, when the pH reaches 7.0, stop adding Aqueous hydrazine hydrate solution, continue to stir for 30 minutes and 4 miles The nano-gold solution with a gold content of 0.76%, the average diameter of the gold particles is 25 nm ° [Simplified illustration] Figure 1 is the x-rays of the nano gold solution prepared at room temperature after drying at 8 ° C Diffraction pattern; ',, Figure 2 is the electron micrograph of nano gold prepared at room temperature; Figure 3 is the diffraction of xenon ray 1275571 taken after the nano gold solution prepared at room temperature is dried at 85 ° C Figure. 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