Electrolysis method: the electrolyte is prepared from ammonium sulfate and sulfuric acid. After impurities are removed, the electrolyte is electrolyzed. HSO4 is discharged at the anode to generate persulfuric acid, and then reacts with ammonium sulfate to generate ammonium persulfate. When the content of ammonium persulfate in the anode solution reaches a certain concentration, the finished ammonium persulfate is prepared through filtration, crystallization, centrifugation and drying.

經(jīng)過除鐵和除雜質(zhì)后的精制電解液，由高位槽連續(xù)進(jìn)入隔膜電解槽，電解液的組成為：陰極液為硫酸280～340kg/m3；硫酸銨180～210kg/m3。陽極液為硫酸110～140kg/m3；硫酸銨300～340kg/m3。通常陽極的電流密度為20～25A/L，槽電壓為5.5～5.8V，電解溫度控制在25～30℃。槽電壓過高，易使已生成的過二硫酸水解成過硫酸而降低電流效率；槽溫過低，易析出過硫酸銨結(jié)晶，堵塞管路。為了提高電流效率，通常添加硫氰酸銨，其量約為電解液的0.015%～0.03%。電解后，陽極液中的過硫酸銨含量應(yīng)達(dá)到220～260kg/m3，收集于陽極液儲(chǔ)槽后，經(jīng)過濾加入結(jié)晶器內(nèi)，在攪拌下，通入冷凍劑進(jìn)行間接冷凍，使過硫酸銨結(jié)晶。待溫度降至-8～-12℃時(shí)，停止冷凍。然后離心分離，再經(jīng)干燥，即得成品。母液循環(huán)使用。電解法的電流效率約為84%～85%。

The refined electrolyte after removing iron and impurities continuously enters the diaphragm electrolyzer from the high-level tank. The composition of the electrolyte is as follows: the cathode liquid is sulfuric acid 280 ～ 340kg/m3; Ammonium sulfate 180 ～ 210kg/m3. The anode solution is sulfuric acid 110 ～ 140kg/m3; Ammonium sulfate 300 ～ 340kg/m3. Generally, the current density of anode is 20~25A/L, the cell voltage is 5.5~5.8V, and the electrolysis temperature is controlled at 25~30 ℃. If the tank voltage is too high, it is easy to hydrolyze the generated persulfuric acid into persulfuric acid and reduce the current efficiency; If the tank temperature is too low, ammonium persulfate crystals are easy to precipitate and block the pipeline. In order to improve the current efficiency, ammonium thiocyanate is usually added, which is about 0.015%~0.03% of the electrolyte. After electrolysis, the content of ammonium persulfate in the anode liquid shall reach 220 ～ 260kg/m3, which shall be collected in the anode liquid storage tank, filtered and added into the crystallizer. Under stirring, the ammonium persulfate shall be indirectly frozen with refrigerant to crystallize. Stop freezing when the temperature drops to - 8~- 12 ℃. After centrifugation and drying, the finished product is obtained. Mother liquor is recycled. The current efficiency of electrolysis is about 84%~85%.

電解硫酸銨的硫酸溶液可制得過二硫酸銨。電解裝置為一放在燒杯中的帶底的容積為80～100mL的素?zé)赏?，素瓷筒?nèi)裝入陽極液，燒杯與素瓷筒之間裝陰極液。鉑絲制成的螺旋狀陽極插入陽極液中，以鉛板制成的圓筒狀的陰極置于素瓷筒外的陰極液中。將硫酸銨溶解在濃度為2mol/L的稀硫酸中制成飽和溶液，并以此溶液為陽極液，陰極液為等體積濃硫酸與水混合形成的稀硫酸溶液。燒杯放在冷水中冷卻，在電解過程中保持陽極液的溫度在10～20℃的范圍內(nèi)。在電流為2～3A下電解一段時(shí)間后，在素瓷筒中即會(huì)有過二硫酸銨的結(jié)晶析出。經(jīng)3～4h后，將陽極液中的全部結(jié)晶取出并用玻璃砂芯漏斗過濾，在40℃以下的溫度下進(jìn)行真空干燥，即可得到過二硫酸銨產(chǎn)品。濾液經(jīng)用硫酸銨飽和后，可再裝入素瓷筒中繼續(xù)電解。經(jīng)2～3次反復(fù)后，陽極液中硫酸過剩較多，可在冷卻的條件下用以硫酸銨飽和的氨水中和部分硫酸。經(jīng)幾次反復(fù)后，陰極液中的硫酸濃度會(huì)大大降低，甚至變?yōu)閴A性，此時(shí)必須更換陰極液，否則電流會(huì)迅速減弱。

Ammonium persulfate can be prepared by electrolyzing the sulfuric acid solution of ammonium sulfate. The electrolysis device is a plain porcelain cylinder with a bottom volume of 80~100mL, which is placed in the beaker. The plain porcelain cylinder is filled with anode liquid, and the cathode liquid is installed between the beaker and the plain porcelain cylinder. The spiral anode made of platinum wire is inserted into the anode liquid, and the cylindrical cathode made of lead plate is placed in the cathode liquid outside the plain porcelain cylinder. Ammonium sulfate is dissolved in dilute sulfuric acid with a concentration of 2mol/L to make a saturated solution, which is used as anode solution and cathode solution as dilute sulfuric acid solution formed by mixing concentrated sulfuric acid with water of equal volume. The beaker is cooled in cold water, and the temperature of the anode liquid is kept within the range of 10-20 ℃ during electrolysis. After electrolysis for a period of time under the current of 2~3A, ammonium persulfate will crystallize in the plain porcelain cylinder. After 3-4 hours, take out all the crystals in the anode solution and filter them with glass sand core funnel, then vacuum dry them at a temperature below 40 ℃ to obtain ammonium persulfate. After the filtrate is saturated with ammonium sulfate, it can be put into a plain porcelain cylinder to continue electrolysis. After 2-3 repetitions, there is more sulfuric acid in the anode solution, and some sulfuric acid can be neutralized with ammonia saturated with ammonium sulfate under cooling conditions. After several repetitions, the concentration of sulfuric acid in the cathode liquid will be greatly reduced, or even become alkaline. At this time, the cathode liquid must be replaced, or the current will rapidly weaken.

制法 將硫酸銨飽和溶液和硫酸混合，濾去不溶物，作為電解液，以鉑作為電極，電解溫度維持在35～45℃為宜，電壓12A 左右，HSO4-子在陽極失電子生成過二硫酸，再與硫酸銨反應(yīng)生成過硫酸銨，總反應(yīng)式為：

In the preparation method, mix the saturated ammonium sulfate solution with sulfuric acid, filter out the insoluble matter, use platinum as the electrode, maintain the electrolysis temperature at 35~45 ℃, and the voltage is about 12A. The HSO4 particle loses electrons at the anode to generate persulfuric acid, and then react with ammonium sulfate to generate ammonium persulfate. The total reaction formula is:

當(dāng)電解液中過硫酸銨達(dá)到一定濃度，調(diào)節(jié)PH＝7～8，然后將電解液過濾，濾液冷卻結(jié)晶，結(jié)晶用少量冷水洗滌至合格后甩干，在40℃以下干燥，得試劑過硫酸銨。

When ammonium persulfate in the electrolyte reaches a certain concentration, adjust PH=7~8, then filter the electrolyte, cool the filtrate for crystallization, wash the crystallization with a small amount of cold water until it is qualified, and then dry it at 40 ℃ to obtain the reagent ammonium persulfate.