CN110482618A - A kind of synthetic method of no nitre chloroplatinic acid - Google Patents
A kind of synthetic method of no nitre chloroplatinic acid Download PDFInfo
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- CN110482618A CN110482618A CN201910745914.3A CN201910745914A CN110482618A CN 110482618 A CN110482618 A CN 110482618A CN 201910745914 A CN201910745914 A CN 201910745914A CN 110482618 A CN110482618 A CN 110482618A
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- chloroplatinic acid
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- C01—INORGANIC CHEMISTRY
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- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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Abstract
The invention discloses a kind of high-efficiency synthesis methods of no nitre chloroplatinic acid, comprising the following steps: (1) the molten platinum powder of chloroazotic acid, (2) activating pretreatment, (3) filtration washing, (4) are synthesized without nitre chloroplatinic acid.The present invention can directly react with hydrochloric acid by activating pretreatment process improving platinum powder reactivity, chloroplatinic acid can be obtained.In addition, the present invention is also by the Optimal improvements of each step reaction condition to crucial preparation method, this method can effectively solve the problem that the exhaust emission of nitrogen oxides in flooding process, product nitrate anion remain serious problem compared with conventional preparation techniques.
Description
Technical field
The invention belongs to the preparation process fields of chloroplatinic acid, and in particular to a kind of high-efficiency synthesis method of no nitre chloroplatinic acid.
Background technique
Chloroplatinic acid is a kind of important compound of noble metal platinum, is widely used in preparing catalyst, plating and prepares it
His platinum-like compounds.
Tradition prepares chloroplatinic acid technique using the molten platinum of chloroazotic acid, then by constantly catching up with nitrate for chloroplatinic acid.
The method, which exists, catches up with nitre activity time long, generates a large amount of discharged nitrous oxides, and also easily there is nitre in product
The problems such as acid group remaining influence product quality.
Summary of the invention
Technical problem to be solved by the present invention lies in for catch up in existing chloroplatinic acid synthetic technology nitre technique repeatedly, nitric acid
The problems such as root removal is not thorough, discharged nitrous oxides, provide it is a kind of it is easy, quickly, discharged nitrous oxides are few, nitrate anion removal rate
High process of preparing.
The technical solution adopted by the present invention to solve the technical problems is: a kind of synthetic method of no nitre chloroplatinic acid, step
It is as follows:
(1) the molten platinum of chloroazotic acid: being added metal platinum into chloroazotic acid according to a certain percentage, and the reaction mixture is heated to 50~
60 DEG C carry out dissolution reaction, until bubble-free generates and stops heating in reaction system, are cooled to room temperature, filter, filtrate is taken to be denoted as the
One product；
(2) pre-treatment and activation: taking the first product to be slowly added into 30% sodium hydroxide solution thereto, adjust solution ph to 9 with
On, solution temperature is maintained at 40~50 DEG C, and reducing agent is then slowly added dropwise, and reducing agent is sodium borohydride, hydrazine hydrate and sulfurous
One or more of sour ammonium mixture adjusts the rate of addition of reducing agent, and control reaction is mild to be carried out, and closes after the reaction was completed
Heating is cooled to room temperature, and obtaining supernatant is colorless and transparent solidliquid mixture, is denoted as the second product；
(3) filtration washing: the second product blowing is filtered to remove mother liquor, and a certain amount of deionized water stirring is added to filter cake and mixes
It closes uniformly, is then filtered to remove filtrate, is cleaned repeatedly to filtrate conductivity less than 10 μ s/cm, filter cake is taken to dry, be denoted as the
Three products；
(4) it synthesizes chloroplatinic acid: third product is added to 36% hydrochloric acid solution according to a certain percentage, open stirring and heating,
It keeps reaction system to be uniformly mixed, a certain amount of hydrogen peroxide is taken to be added slowly in reaction system, completely rear continuation to be added is anti-
Certain time is answered, stops heating and is cooled to room temperature, filter, take filtrate to be denoted as the 4th product, by the 4th product according to different clients
It is required that being evaporated concentration, chloroplatinic acid product is obtained.
A kind of synthetic method of no nitre chloroplatinic acid, chloroazotic acid is ready-to-use in step (1), and metal platinum adds with chloroazotic acid
Adding ratio is 1g:3.52~17.6mL.
A kind of synthetic method of no nitre chloroplatinic acid, metal platinum is high-purity platinum in step (1), platinum content >=
99.95%。
A kind of synthetic method of no nitre chloroplatinic acid, feed ratio is reducing agent: metal platinum=1g in step (2):
3g~10g.
A kind of synthetic method of no nitre chloroplatinic acid, filtration washing is washed every time using vacuum filtration in step (3)
Washing water consumption is 2 times of filter cake amounts, is uniformly mixed by mechanical stirring.
A kind of synthetic method of no nitre chloroplatinic acid, third product and hydrochloric acid adding proportion are 1g in step (4):
10~15mL, hydrogen peroxide and hydrochloric acid volume ratio are 1:1~7, and charging rate is 10~100mL/min, and initial reaction temperature is
30~90 DEG C.
A kind of synthetic method of no nitre chloroplatinic acid, it is pure that the above-mentioned raw material used are all made of analysis.
The beneficial effects of the present invention are: the present invention is removed using the activated pretreating process of high-purity platinum, filter and cleaning process
Foreign ion, obtaining highly pure active platinum powder can directly react to obtain platinum acid chloride solution with hydrochloric acid, eliminate in traditional handicraft repeatedly
Nitre process is caught up with, discharged nitrous oxides are reduced, and solves the problems, such as to realize nothing because of the nitrate anion residual for catching up with nitre to be not thorough generation
The preparation of nitre chloroplatinic acid product.
Detailed description of the invention
Fig. 1 is preparation method flow chart of the invention.
Specific embodiment
A kind of preparation method of chloroplatinic acid disclosed by the invention, specially by platinum powder pre-treatment and activation, washing impurity-removing, then
It is redissolved, is concentrated to get chloroplatinic acid product.As shown in Figure 1, the basic principle used is four step synthetic methods, the first step by platinum powder with
Aqua regia dissolution's reaction is prepared the first product, and second step will be in the first product and reduction obtain the second product, and third step is by the
Three product filtration washings remove foreign ion, drying obtains third product, and the 4th step reacts third product with hydrochloric acid to obtain chlorine
Platinic acid solution obtains chloroplatinic acid product through being concentrated by evaporation according to customer requirement.Wherein
Below by specific embodiment, the present invention will be further described, but protection scope is not limited by these examples of implementation.
Embodiment 1
10g platinum powder is taken to be placed in flask, separately according to platinum powder: chloroazotic acid=1g:4.5mL is added chloroazotic acid and opens stirring, maintains the temperature at
50 DEG C start dissolution reaction, stop heating after 3h, are cooled to room temperature filtering, filtrate is taken to obtain the first product, platinum powder dissolution rate is
90%。
30% sodium hydroxide solution is added into the first obtained product under agitation, adjusts solution ph to 10.It opens
Opening heating makes solution temperature be maintained at 50 DEG C, and hydrazine hydrate solution is then slowly added dropwise thereto, careful to control hydrazine hydrate charging speed
Degree avoids reaction from excessively acutely occurring emitting kettle.Continue to be stirred to react 1h after hydrazine hydrate is added dropwise to complete, closes heating, be cooled to room
Temperature, obtaining supernatant is the second colorless and transparent product.
The second obtained product is removed into mother liquor through vacuum filter, the deionization of 2 times of filter cake amounts is then added into filter cake
Water is thoroughly mixed uniformly, filters and remove filtrate, washs 5 times repeatedly, until filtrate conductivity is 7 μ s/cm.It will obtain
Filter cake be put into 80 DEG C of baking ovens dry 12h and obtain third product.
Third product is placed in reaction flask, 36% hydrochloric acid solution 120mL is added, open stirring and is heated reactant
It is that temperature is maintained at 50 DEG C, adds 30% hydrogen peroxide solution 60mL followed by peristaltic pump, control charging rate is 20mL/min,
Hydrogen peroxide continues to stop heating and stirring after being stirred to react 1h after being added dropwise to complete, and is cooled to room temperature rear blowing filtering, and dissolution rate is
93%.Obtained filtrate is concentrated by evaporation according to customer requirement to 80g/L and obtains platinum acid chloride solution product.
Embodiment 2
10g platinum powder is taken to be placed in flask, separately according to platinum powder: chloroazotic acid=1g:7.5mL is added chloroazotic acid and opens stirring, maintains the temperature at
60 DEG C start dissolution reaction, stop heating after 3h, are cooled to room temperature filtering, filtrate is taken to obtain the first product, platinum powder dissolution rate connects
Nearly 100%.
30% sodium hydroxide solution is added into the first obtained product under agitation, adjusts solution ph to 12.It opens
Opening heating makes solution temperature be maintained at 40 DEG C, and sodium borohydride solution is then slowly added dropwise thereto, and the careful sodium borohydride that controls adds
Material speed avoids reaction from excessively acutely occurring emitting kettle.Continue to be stirred to react 1h after sodium borohydride is added dropwise to complete, closes heating, it is cold
But to room temperature, obtaining supernatant is the second colorless and transparent product.
The second obtained product is removed into mother liquor through vacuum filter, the deionization of 2 times of filter cake amounts is then added into filter cake
Water is thoroughly mixed uniformly, filters and remove filtrate, washs 7 times repeatedly, until filtrate conductivity is 7 μ s/cm.It will obtain
Filter cake be put into 80 DEG C of baking ovens dry 12h and obtain third product.
Third product is placed in reaction flask, 36% hydrochloric acid solution 140mL is added, open stirring and is heated reactant
It is that temperature is maintained at 70 DEG C, adds 30% hydrogen peroxide solution 60mL followed by peristaltic pump, control charging rate is 10mL/min,
Hydrogen peroxide continues to stop heating and stirring after being stirred to react 1h after being added dropwise to complete, and is cooled to room temperature rear blowing filtering, and dissolution rate is
99%.Obtained filtrate is concentrated by evaporation according to customer requirement to 120g/L and obtains platinum acid chloride solution product.
The above-described embodiments merely illustrate the principles and effects of the present invention, and the embodiment that part uses, for
For those skilled in the art, without departing from the concept of the premise of the invention, can also make it is several deformation and
It improves, these are all within the scope of protection of the present invention.
Claims (7)
1. a kind of synthetic method of no nitre chloroplatinic acid, it is characterised in that: include the following steps
(1) the molten platinum of chloroazotic acid: being added metal platinum into chloroazotic acid in proportion, maintains the temperature at 50~60 DEG C and carries out dissolution reaction, until anti-
It answers bubble-free in system to generate stopping heating, is cooled to room temperature, filters, filtrate is taken to be denoted as the first product；
(2) pre-treatment and activation: being slowly added into 30% sodium hydroxide solution into the first product, adjusts solution ph to 9 or more,
Solution temperature is maintained at 40~50 DEG C, and reducing agent is then slowly added dropwise, and reducing agent is sodium borohydride, hydrazine hydrate and ammonium sulfite
One or more of mixture, after the reaction was completed, close heating be cooled to room temperature, obtain supernatant be colorless and transparent solid-liquid
Mixture is denoted as the second product；
(3) filtration washing: being filtered to remove mother liquor for the second product blowing, and deionized water be added to filter cake and is uniformly mixed,
Then it is filtered to remove filtrate, is cleaned repeatedly to filtrate conductivity less than 10 μ s/cm, is taken filter cake to dry, be denoted as third product；
(4) it synthesizes chloroplatinic acid: 36% hydrochloric acid solution being added into third product, agitating and heating keeps reaction system mixing equal
It is even, take hydrogen peroxide to be slowly added into, reaction certain time stops heating and is cooled to room temperature, and filters, filtrate is taken to be denoted as the 4th product, will
4th product is evaporated concentration, obtains chloroplatinic acid product.
2. a kind of synthetic method of no nitre chloroplatinic acid according to claim 1, which is characterized in that king in the step (1)
Water is ready-to-use, and metal platinum and chloroazotic acid adding proportion are 1g:3.52~17.6mL.
3. a kind of synthetic method of no nitre chloroplatinic acid according to claim 1, which is characterized in that golden in the step (1)
Category platinum is high-purity platinum, platinum content >=99.95%.
4. a kind of synthetic method of no nitre chloroplatinic acid according to claim 1, which is characterized in that add in the step (2)
Material ratio is reducing agent: metal platinum=1g:3g~10g.
5. a kind of synthetic method of no nitre chloroplatinic acid according to claim 1, which is characterized in that mistake in the step (3)
Using vacuum filtration, each slurry amount is 2 times of filter cake amounts for filter washing, is uniformly mixed by mechanical stirring.
6. a kind of synthetic method of no nitre chloroplatinic acid according to claim 1, which is characterized in that in the step (4)
Three products and hydrochloric acid adding proportion are 1g:10~15mL, and hydrogen peroxide and hydrochloric acid volume ratio are 1:1~7, charging rate is 10~
100mL/min, initial reaction temperature are 30~90 DEG C.
7. according to claim 1 to a kind of synthetic method of no nitre chloroplatinic acid described in 6 Arbitrary Terms, which is characterized in that above-mentioned original
It is pure that material is all made of analysis.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929158A (en) * | 2021-10-28 | 2022-01-14 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
| CN114735766A (en) * | 2022-04-07 | 2022-07-12 | 安徽枡水新能源科技有限公司 | Preparation method of nitrate-free chloroplatinic acid without introducing sodium ion impurities |
| CN115477340A (en) * | 2022-08-18 | 2022-12-16 | 山东有研国晶辉新材料有限公司 | Preparation method of chloroplatinic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
| CN108907217A (en) * | 2018-07-27 | 2018-11-30 | 江苏北矿金属循环利用科技有限公司 | A kind of method that short route prepares Ultrafine Platinum Powder |
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2019
- 2019-08-13 CN CN201910745914.3A patent/CN110482618A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370845A (en) * | 2001-10-09 | 2002-09-25 | 金川集团有限公司 | Refined platinum producing process |
| CN108655415A (en) * | 2018-06-20 | 2018-10-16 | 南京东锐铂业有限公司 | A kind of new process preparing high-purity platinum |
| CN108907217A (en) * | 2018-07-27 | 2018-11-30 | 江苏北矿金属循环利用科技有限公司 | A kind of method that short route prepares Ultrafine Platinum Powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113929158A (en) * | 2021-10-28 | 2022-01-14 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
| CN113929158B (en) * | 2021-10-28 | 2023-10-03 | 浙江微通催化新材料有限公司 | Preparation method of platinum nitrate |
| CN114735766A (en) * | 2022-04-07 | 2022-07-12 | 安徽枡水新能源科技有限公司 | Preparation method of nitrate-free chloroplatinic acid without introducing sodium ion impurities |
| CN115477340A (en) * | 2022-08-18 | 2022-12-16 | 山东有研国晶辉新材料有限公司 | Preparation method of chloroplatinic acid |
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Application publication date: 20191122 |