CN102660684A - Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate - Google Patents
Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate Download PDFInfo
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- CN102660684A CN102660684A CN2012101154258A CN201210115425A CN102660684A CN 102660684 A CN102660684 A CN 102660684A CN 2012101154258 A CN2012101154258 A CN 2012101154258A CN 201210115425 A CN201210115425 A CN 201210115425A CN 102660684 A CN102660684 A CN 102660684A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for extracting crude silver by using wastewater of a silver plating production line of rhinestone as a raw material and refining the crude silver to pure silver. Besides, in order to reuse the silver in the silver plating production line, the invention further provides a method for preparing the refined pure silver to a silver nitrate solution and afterwards preparing crude silver nitrate then fine silver nitrate. Compared with the prior method for treating the wastewater produced during silver plating of the rhinestone, the methods fill the gap in silver-containing wastewater treatment of the rhinestone industry. Noble metal silver is fully recovered from the wastewater of the silver plating production line of the rhinestone and purified to prepare the high-purity silver nitrate, so that the use requirement of the silver plating production line is met, the silver is repeatedly utilized and the cost is saved.
Description
Technical field
The invention belongs to the Industrial Wastewater Treatment field, specifically, relate to a kind of treating water and bore Silver Electroplating Production Line waste water, the silver and prepare the method for high purity silver nitrate of purifying.
Background technology
It is a kind of ornaments auxiliary that becomes the diamond facet to obtain the synthetic quartz glass cutting that water bores, and water bores material economy, and the brilliant sensation as the diamond is arranged again on the visual effect simultaneously.Therefore in low and middle-grade ornaments designs, be widely used.
Water bores in the production process can produce more silver-containing waste water, as changing plating Silver Nitrate waste water, deposited silver mud etc.; Owing to contain precious metal silver, therefore handle waste water, purification silver wherein, and with precious metal silver purifying and preparing high-purity Silver Nitrate; Reach the Silver Electroplating Production Line request for utilization; Cost is saved in recycling, is of great value work.
At present; The silver method commonly used of from silver-containing waste water, purifying has ion exchange method, chemical precipitation method etc.; A kind of method of the silver of from film rinsing waste water, purifying is disclosed like Chinese patent CN86100283B; CN1394973 also discloses a kind of method of handling the argentiferous waste material, utilizes wet method-pyrogenic attack silver content to be lower than 3% waste material; But do not mention that all how to bore factory effluent to water extracts also purifying noble metal silver.In addition; Chinese patent CN1073412 and CN1386707 have introduced how to remove to produce high purity silver nitrate with high fine silver, and the waste gas waste water in the production process is handled, but collected useless silver all is thick silver in actual production; Can not directly be used to produce Silver Nitrate, certain limitation is arranged.
Because the silver that water bores in the silver-containing waste water that industry produced is cotton-shaped, be difficult to collect, and foreign matter content is high, be difficult to recycle useless silver, also there is not effective means to handle recovery at present.
So to above-mentioned defective, the present invention has highlighted and bored Silver Electroplating Production Line waste water like water how is raw material, extracts thick silver, and will thick silver refines and be fine silver, then fine silver is prepared into the method for high purity silver nitrate.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with water brill Silver Electroplating Production Line waste water, extract slightly silver, and slightly the silver refinement is the method for fine silver.
Simultaneously, the present invention also provides the method that above-mentioned fine silver is prepared into high purity silver nitrate, and said Silver Nitrate can be back to water and bore Silver Electroplating Production Line.
Generally, water bores Silver Electroplating Production Line waste water and mainly contains glucose, sodium hydroxide, and tin protochloride, cotton-shaped sponge silver, formaldehyde etc., silver content is about about 20%.
Of the present invention is raw material with water brill Silver Electroplating Production Line waste water, extract slightly silver, and slightly the silver refinement is to may further comprise the steps the method for fine silver:
1) reclaims thick silver: Silver Electroplating Production Line waste water is drained into settling tank; Press waste water: the mass ratio of water purification agent=1000: 1-6 drops into water purification agent, static 12-24 hour, treats that supernatant liquid carries out solid-liquid separation after as clear as crystal; With the solid drying of gained, promptly obtain containing the thick silver of water purification agent;
2) thick silver refines fine silver: will contain thick silver and borax, yellow soda ash and the SODIUMNITRATE premix of water purification agent, and continue calcination 1-2 hour more than 1000 ℃ then, and add borax or SODIUMNITRATE according to thick silver-colored dissolving situation during the calcination; Melt into liquid, will mix thick silver-colored mixtures of liquids then and pour mould into, leave standstill cooling; Until the upper strata is impurity; Lower floor is a fine silver, and silver bullion is taken out, and obtains fine silver; Wherein, the mass ratio that said premix adds borax, yellow soda ash and the SODIUMNITRATE of thick silver is 1: 1: 1, and total mass is no more than thick silver amount 3%; The add-on of said borax or SODIUMNITRATE is no more than thick silver amount 2%.
Said settling tank can be the fractionation precipitation pond, and said fractionation precipitation pond can be made up of 3-5 settling tank;
Said water purification agent can adopt this area water purification agent commonly used, preferred polymeric aluminum chloride, and alum, one or more in the Tai-Ace S 150,
The preferred waste water of the add-on of said water purification agent: the mass ratio of water purification agent=1000: 3-5; More preferably waste water: the mass ratio of water purification agent=1000: 5;
Preferred 24 hours of said rest time;
Said solid-liquid separation can adopt this area method commonly used; As centrifugal, filtration, press filtration etc.; The preferred centrifuging that adopts is carried out, and solid is dried with whizzer, obtains containing the thick silver of water purification agent.
Said calcination can adopt this area equipment commonly used to carry out, and like the air blast coke-fired furnace etc., the temperature of calcination generally is no more than 250 ℃ of fine silver fusing points.
The total mass that said premix adds borax, yellow soda ash and the SODIUMNITRATE of thick silver is generally 0.5-3%.In the calcination process, the add-on of said borax or SODIUMNITRATE is generally 0-2%.
For obtain can reuse high purity silver nitrate, method of the present invention also comprises the method that fine silver is prepared as Silver Nitrate.
Said method is in above-mentioned steps 2) after, also comprise:
3) preparation silver nitrate solution: in silver bullion, add nitric acid, silver is 1 with the mass ratio of nitric acid: 0.8-1.2; Be warming up to 80-90 ℃ then, be incubated 8-12 hour, adding quality is the gac of silver bullion quality 1 ‰-5 ‰, filters then and obtains silver nitrate solution;
4) preparation crude silver nitrate solid: silver nitrate solution is carried out normal pressure or underpressure distillation, obtain the crude silver nitrate solid;
5) refining Silver Nitrate: in crude silver nitrate, add ultrapure water, the mass ratio of ultrapure water and Silver Nitrate is 1: 0.8-1.2, rising temperature for dissolving; Adding quality is silver bullion quality 1 ‰-5 ‰ gac; 78-85 ℃ of insulation 1-2 hour, filter and obtain silver nitrate solution, then silver nitrate solution is carried out normal pressure or underpressure distillation; Obtain high purity silver nitrate, can supply silvering shop to use after the oven dry.
In the step 3), it is the salpeter solution of 58-65% that said nitric acid adopts mass concentration, and the add-on of nitric acid is a radix with the quality of salpeter solution, and preferred mass concentration is 63% nitric acid; The mass ratio of said silver and nitric acid is preferably 1: 1; Preferred 85 ℃ of said temperature; Said normal pressure or underpressure distillation are carried out in still kettle; The general pressure that adopts is-below the 0.1MPa; Waste gas absorbs through the absorption tower, and the 10%NaOH solution of absorption agent for down spraying from cat head adopts the centrifugal exhaust fan exhausting to form negative pressure;
In the step 5), said making with extra care in refining kettle carried out; The mass ratio of said ultrapure water and Silver Nitrate is preferably 1: 1; Preferred 80 ℃ of said temperature.
Bore the method for silver-plated factory effluent compares with existing treating water; The present invention has filled up water and has bored the blank that the industry silver-containing waste water is handled; Bore the abundant precious metal silver that reclaims the Silver Electroplating Production Line waste water from water, and, reach the Silver Electroplating Production Line request for utilization precious metal silver purifying and preparing high-purity Silver Nitrate; Cost is saved in recycling.
Description of drawings
Fig. 1 is a kind of schema that utilizes water to bore Silver Electroplating Production Line waste water purification silver and prepare the method for high purity silver nitrate of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is described further.Specialize like nothing, the used raw material of the present invention is commercial.Wherein utilize water to bore purify silver and to prepare the flow process of method of high purity silver nitrate as shown in Figure 1 of Silver Electroplating Production Line waste water in the various embodiments of the present invention.
Embodiment 1
Water bores Silver Electroplating Production Line waste water and mainly contains glucose, sodium hydroxide, tin protochloride, cotton-shaped sponge silver, formaldehyde etc., thick silver-colored silver content about 20%.
Water bores slightly silver of Silver Electroplating Production Line waste water reclamation.The waste water that Silver Electroplating Production Line produces drains into the fractionation precipitation pond and precipitates; This settling tank is made up of 3 settling tanks; Drop into the water purification agent Poly aluminum Chloride (PAC) by concentration 5 ‰, static 24 hours, carry out solid-liquid separation after the time supernatant liquid is as clear as crystal; Solid dries with whizzer, obtains containing the thick silver-colored 100kg of water purification agent.
Thick silver refines fine silver.With thick silver and borax, yellow soda ash and SODIUMNITRATE premix, wherein the mass ratio of borax, yellow soda ash and SODIUMNITRATE is 1: 1: 1, and total mass is thick silver amount 3%; Put into crucible then, crucible is put into the air blast coke-fired furnace be warming up to more than 1000 ℃, continue calcination 1.5 hours; The melting state of thick silver continues to add separately borax to quicken thick silver dissolving (add-on of borax is thick silver amount 2%) during then according to melting, treats that thick silver is melted into liquid in the crucible, then liquid is poured in the irony grinding tool; The upper strata is an impurity; Lower floor is a fine silver, after the cooling silver bullion is taken out a little, obtains fine silver 20kg.
Prepare high purity silver nitrate by fine silver.Silver bullion is dropped in the stainless steel cauldron, and the nitric acid of weight such as adding (mass concentration 63%) is warming up to 85 ℃; Be incubated 12 hours; Add 1 ‰ gac, filter then and obtain silver nitrate solution, join and carry out air distillation in the still kettle; Waste gas absorbs through the absorption tower, obtains crude silver nitrate 31.48kg.
Crude silver nitrate put in the refining kettle make with extra care; The ultrapure water of weight such as adding and Silver Nitrate, rising temperature for dissolving adds 1 ‰ gacs 80 ℃ of insulations 1 hour; Filtration obtains silver nitrate solution; Join in the still kettle and distill, obtain high purity silver nitrate 20Kg, can supply silvering shop to use after the oven dry bottling.The mother liquor that simultaneously, will contain high density Silver Nitrate and partial impurities joins recycled in the preparation crude silver nitrate operation.
Embodiment 2
Water bores slightly silver of Silver Electroplating Production Line waste water reclamation.The waste water that Silver Electroplating Production Line produces drains into the fractionation precipitation pond and precipitates; This settling tank is made up of 5 settling tanks; Drop into the water purification agent Poly aluminum Chloride (PAC) by concentration 3 ‰, static 20 hours, carry out solid-liquid separation after the time supernatant liquid is as clear as crystal; Solid dries with whizzer, obtains containing the thick silver-colored 100kg of water purification agent.
Thick silver refines fine silver.With thick silver and borax, yellow soda ash and SODIUMNITRATE premix, wherein the mass ratio of borax, yellow soda ash and SODIUMNITRATE is 1: 1: 1, and total mass is thick silver amount 1.5%; Put into crucible then, crucible is put into the air blast coke-fired furnace be warming up to 1100 ℃, continue calcination 2 hours; The melting state of thick silver continues to add separately SODIUMNITRATE to quicken thick silver dissolving (add-on of SODIUMNITRATE is thick silver amount 1.5%) during according to melting, treats that thick silver is melted into liquid in the crucible, then liquid is poured in the irony grinding tool; The upper strata is an impurity; Lower floor is a fine silver, after the cooling silver bullion is taken out a little, obtains fine silver 20kg.
Prepare high purity silver nitrate by fine silver.Silver bullion is dropped in the stainless steel cauldron, add the nitric acid (mass concentration 63%) of 0.8 times of quality of silver bullion quality, be warming up to 80 ℃; Be incubated 8 hours; Add 3 ‰ gac, filter then and obtain silver nitrate solution, join and carry out air distillation in the still kettle; Waste gas absorbs through the absorption tower, obtains crude silver nitrate 31.48kg.
Crude silver nitrate put in the refining kettle make with extra care; The ultrapure water of adding and 1.2 times of quality of Silver Nitrate weight, rising temperature for dissolving adds 3 ‰ gacs 85 ℃ of insulations 1 hour; Filtration obtains silver nitrate solution; Join in the still kettle and distill, obtain high purity silver nitrate 20kg, can supply silvering shop to use after the oven dry bottling.
The mother liquor that simultaneously, will contain high density Silver Nitrate and partial impurities joins recycled in the preparation crude silver nitrate operation.
Embodiment 3
Water bores slightly silver of Silver Electroplating Production Line waste water reclamation.The waste water that Silver Electroplating Production Line produces drains into the fractionation precipitation pond and precipitates; This settling tank is made up of 3 settling tanks; Drop into the water purification agent Poly aluminum Chloride (PAC) by concentration 4 ‰, static 12 hours, carry out solid-liquid separation after the time supernatant liquid is as clear as crystal; Solid dries with whizzer, obtains containing the thick silver-colored 100kg of water purification agent.
Thick silver refines fine silver.With thick silver and borax, yellow soda ash and SODIUMNITRATE premix, wherein the mass ratio of borax, yellow soda ash and SODIUMNITRATE is 1: 1: 1, and total mass is thick silver amount 1%; Put into crucible then, crucible is put into the air blast coke-fired furnace be warming up to 1050 ℃, continue calcination 1 hour; The melting state of thick silver continues to add separately borax to quicken thick silver dissolving (add-on of borax is thick silver amount 1.0%) during according to melting, treats that thick silver is melted into liquid in the crucible, then liquid is poured in the irony grinding tool; The upper strata is an impurity; Lower floor is a fine silver, after the cooling silver bullion is taken out a little, obtains fine silver 20kg.
Prepare high purity silver nitrate by fine silver.Silver bullion is dropped in the stainless steel cauldron, and the nitric acid of weight such as adding is warming up to 82 ℃; Be incubated 10 hours, add 5 ‰ gac, filter then and obtain silver nitrate solution; Join and carry out air distillation in the still kettle, waste gas absorbs through the absorption tower, obtains crude silver nitrate 31.48kg.
Crude silver nitrate put in the refining kettle make with extra care; The ultrapure water of weight such as adding and Silver Nitrate, rising temperature for dissolving adds 5 ‰ gacs 85 ℃ of insulations 1 hour; Filtration obtains silver nitrate solution; Join in the still kettle and distill, obtain high purity silver nitrate 20kg, can supply silvering shop to use after the oven dry bottling.
The mother liquor that simultaneously, will contain high density Silver Nitrate and partial impurities joins recycled in the preparation crude silver nitrate operation.
Claims (10)
1. one kind is utilized water to bore the purify method of silver of Silver Electroplating Production Line waste water, and boring Silver Electroplating Production Line waste water with water is raw material, extracts thick silver, and will thick silver refines and be fine silver, it is characterized in that, may further comprise the steps:
1) reclaims thick silver: Silver Electroplating Production Line waste water is drained into settling tank; Press waste water: the mass ratio of water purification agent=1000: 1-6 drops into water purification agent, static 12-24 hour, treats that supernatant liquid carries out solid-liquid separation after as clear as crystal; With the solid drying of gained, promptly obtain containing the thick silver of water purification agent;
2) thick silver refines fine silver: will contain thick silver and borax, yellow soda ash and the SODIUMNITRATE premix of water purification agent, and continue calcination 1-2 hour more than 1000 ℃ then, and add borax or SODIUMNITRATE according to thick silver-colored dissolving situation during the calcination; Melt into liquid, will mix thick silver-colored mixtures of liquids then and pour mould into, leave standstill cooling; Until the upper strata is impurity; Lower floor is a fine silver, and silver bullion is taken out, and obtains fine silver; Wherein, the mass ratio that said premix adds borax, yellow soda ash and the SODIUMNITRATE of thick silver is 1: 1: 1, and total mass is no more than thick silver amount 3%; The add-on of said borax or SODIUMNITRATE is no more than thick silver amount 2%.
2. method according to claim 1 is characterized in that, in the step 1), said settling tank can be the fractionation precipitation pond, and said fractionation precipitation pond can be made up of 3-5 settling tank.
3. method according to claim 1 is characterized in that, in the step 1), said solid-liquid separation adopts centrifuging to carry out.
4. method according to claim 1 is characterized in that, in the step 1), said water purification agent is a Poly aluminum Chloride (PAC), alum, one or more in the Tai-Ace S 150.
5. method according to claim 1 is characterized in that, in the step 1), the add-on of said water purification agent is a waste water: the mass ratio of water purification agent=1000: 3-5; Preferred waste water: the mass ratio of water purification agent=1000: 5.
6. one kind is utilized water to bore the method that Silver Electroplating Production Line waste water prepares high purity silver nitrate, and boring Silver Electroplating Production Line waste water with water is raw material, is prepared into high purity silver nitrate; It is characterized in that; Comprise aforesaid right requirement 1 said method, in the step 2 of said method) after, also comprise:
3) preparation silver nitrate solution: in silver bullion, add nitric acid, silver is 1 with the mass ratio of nitric acid: 0.8-1.2; Be warming up to 80-90 ℃ then, be incubated 8-12 hour, adding quality is the gac of silver bullion quality 1 ‰-5 ‰, filters then and obtains silver nitrate solution;
4) preparation crude silver nitrate solid: silver nitrate solution is carried out normal pressure or underpressure distillation, obtain the crude silver nitrate solid;
5) refining Silver Nitrate: in crude silver nitrate, add ultrapure water; The mass ratio of ultrapure water and Silver Nitrate is 1: 0.8-1.2, and rising temperature for dissolving, adding quality is silver bullion quality 1 ‰-5 ‰ gac; 78-85 ℃ of insulation 1-2 hour; Filtration obtains silver nitrate solution, then silver nitrate solution is carried out normal pressure or underpressure distillation, obtains high purity silver nitrate.
7. method according to claim 6 is characterized in that, in the step 3), it is the salpeter solution of 58-65% that said nitric acid adopts mass concentration; The mass ratio of said silver and nitric acid is 1: 1.
8. method according to claim 7 is characterized in that, in the step 3), said temperature is 85 ℃.
9. method according to claim 6 is characterized in that, in the step 5), the mass ratio of said ultrapure water and Silver Nitrate is 1: 1.
10. method according to claim 6 is characterized in that, in the step 5), said temperature is 80 ℃.
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| CN2012101154258A CN102660684B (en) | 2012-04-18 | 2012-04-18 | Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate |
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| CN2012101154258A CN102660684B (en) | 2012-04-18 | 2012-04-18 | Method for purifying silver by using wastewater of silver plating production line of rhinestone and method for preparing high-purity silver nitrate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274448A (en) * | 2013-06-19 | 2013-09-04 | 太仓沪试试剂有限公司 | Silver nitrate purifying method |
| CN106044839A (en) * | 2016-08-23 | 2016-10-26 | 太仓沪试试剂有限公司 | Silver nitrate purification method |
| CN107365912A (en) * | 2017-08-01 | 2017-11-21 | 安徽富村微量元素科技有限公司 | Silver come off liquid and from useless glass liner reclaim silver method |
| CN113293298A (en) * | 2021-04-21 | 2021-08-24 | 陕西黄金集团西安秦金有限责任公司 | Method for recovering gold and silver in clay graphite crucible |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828854A (en) * | 2015-04-23 | 2015-08-12 | 金川集团股份有限公司 | Method for preparing high purity silver nitrate from crude silver powder |
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| JPS5311815A (en) * | 1976-07-21 | 1978-02-02 | Mitsubishi Metal Corp | Silver recovering method from extraction residue of wet process zinc smelting |
| CN1118015A (en) * | 1993-11-18 | 1996-03-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from micro-silver contained waste liquid |
| CN102071319A (en) * | 2010-12-16 | 2011-05-25 | 惠州市奥美特环境科技有限公司 | Method for preparing high-purity silver from silver-containing waste liquid |
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Patent Citations (3)
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| JPS5311815A (en) * | 1976-07-21 | 1978-02-02 | Mitsubishi Metal Corp | Silver recovering method from extraction residue of wet process zinc smelting |
| CN1118015A (en) * | 1993-11-18 | 1996-03-06 | 中国有色金属工业总公司昆明贵金属研究所 | Method for recovering silver from micro-silver contained waste liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274448A (en) * | 2013-06-19 | 2013-09-04 | 太仓沪试试剂有限公司 | Silver nitrate purifying method |
| CN106044839A (en) * | 2016-08-23 | 2016-10-26 | 太仓沪试试剂有限公司 | Silver nitrate purification method |
| CN107365912A (en) * | 2017-08-01 | 2017-11-21 | 安徽富村微量元素科技有限公司 | Silver come off liquid and from useless glass liner reclaim silver method |
| CN113293298A (en) * | 2021-04-21 | 2021-08-24 | 陕西黄金集团西安秦金有限责任公司 | Method for recovering gold and silver in clay graphite crucible |
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| CN102660684B (en) | 2013-07-31 |
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Effective date of registration: 20151228 Address after: 321016, Zhejiang Province, Wucheng District, Jinhua Road, 333 fairy Road, 4 building, two floor, Room 201 on the east side Patentee after: JINHUA JINCAN CRYSTAL CO., LTD. Address before: 321016, 333, Yuen Yuan Road, Zhejiang, Jinhua Patentee before: Jinhua Guanhua Crystal Co.,Ltd. |
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Effective date of registration: 20170613 Address after: 325100, No. 15, South Bank Road, welfare Town, Yongjia County, Wenzhou, Zhejiang Patentee after: Pan Xiao Address before: 321016, Zhejiang Province, Wucheng District, Jinhua Road, 333 fairy Road, 4 building, two floor, Room 201 on the east side Patentee before: JINHUA JINCAN CRYSTAL CO., LTD. |