CN106430333A - Palladium chloride production technology - Google Patents
Palladium chloride production technology Download PDFInfo
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- CN106430333A CN106430333A CN201610763052.3A CN201610763052A CN106430333A CN 106430333 A CN106430333 A CN 106430333A CN 201610763052 A CN201610763052 A CN 201610763052A CN 106430333 A CN106430333 A CN 106430333A
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- palladium
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- bichloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/005—Halides
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Abstract
The invention relates to a palladium chloride production technology and belongs to the technical field of chemical industry. The technology comprises four steps as follows: 1, aqua regia dissolution and concentration for nitrate removal; 2, regulation of concentration and pH of a palladium solution; 3, dispersing; 4, spray drying. By means of regulation of the concentration and acidity of the solution and utilization of a dispersing solvent and with the adoption of spray drying equipment for spray drying, the problem of metal loss caused by the fact that a current traditional technology is relatively long in time and has multiple production steps is solved, and meanwhile, the problem of residues of the added dispersing agent in a product is solved, so that the palladium chloride product meets the national standard. Compared with the traditional technology, steps of concentration, crystallization and ball milling are not needed, and obtained product batches are stable; compared with the traditional technology, the loss can be reduced by at least 60%. The content of Pd in the prepared product is higher than or equal to 59.8%, solubility in acid is good, product granularity is -120 meshes, and the requirements of the national standard GB/T8185-2004 are met.
Description
Technical field
The invention belongs to metal in Chemical Manufacture and sort technical field, be specifically related to the production technology of a kind of palladium bichloride.
Background technology
With the development of China's manufacture level, the selectivity that palladium catalyst is had, stability, catalysis activity
Require also to improve constantly.The palladium compound product being commonly used as presoma at present is mainly palladium bichloride.This product is widely used in
Petrochemical industry, medical industry, perfume industry, dye industry, environment-protection wastewater, waste gas, purifying vehicle exhaust and other fine chemistry industries
In catalytic hydrogenation field and electro-catalysis field, the consumption of current Domestic Palladium catalyst converts into palladium meter and has reached 30 tons/year.Work
Industry palladium catalyst can be divided into two classes, and one is homogeneous catalyst i.e. types of functionality palladium compound, Typical Representative such as palladium；Two
Being supported catalyst, such as palladium charcoal, palladium aluminum oxide etc., auto-exhaust catalyst is i.e. one of them（The compound oxidizings such as palladium rhodium
Alumina supporter catalyst）, other also have disproportionated rosin palladium carbon catalyst, hydrogen peroxide industrial palladium aluminium oxide catalyst etc..It is state
Interior most commonly used palladium catalyst presoma.The traditional processing technology of current domestic palladium bichloride is：
.
Owing to technics comparing long production step will result in the loss of metal more in traditional processing technology, also can make simultaneously
Becoming product batches unstable, cost is high.In addition, in the industrial production, the chlorination that obtains after condensing crystallizing in traditional processing technology
Palladium product is mostly for bulk, it is necessary to through ball milling, just can obtain powder.
Although crystalline product being dried disclosed in now many patents and just can obtaining powder, but these patents are substantially all
It is the miniature meeting small-scale test in experiment, and really not so in the industrial production.In the industrial production, but dry after product
Substantially bulk, needs to carry out ball milling, just can obtain powder-product.
Present patent application, for above-mentioned condition, is carried out the production Technology research and development of palladium bichloride, can be realized continuously to obtain
Metaplasia is produced, and product batches is stable, reduces production craft step, reduces the production and processing technology of metal loss, is palladium catalyst row
Industry offer is more reliable, use more convenient persursor material, extends rare precious metal industry industrial chain, fills a hole in the market,
Promote industry development.
Content of the invention
The problems referred to above existing for current palladium bichloride, the present invention provides that a kind of technique is simple, with short production cycle, cost
Low, free from environmental pollution, acid-soluble good, the production technology of the stable palladium bichloride of palladium content.
For achieving the above object, the technical solution used in the present invention is as follows：
The production technology of a kind of palladium bichloride, it is characterised in that comprise the steps：
Step（1）, nitre is caught up with in aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with in concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH regulation：
By step（1）The palladium solution regulation obtaining is 79-81g/L to the concentration of palladium, and pH value is 0.9-1.1；
Step（3）, dispersion：
To through step（2）Adding dispersion solvent in the palladium solution of regulation, the volume that dispersion solvent adds is palladium liquor capacity
4.9-5.1%, the palladium solution after being disperseed；Described dispersion solvent is the mixture of ethanol and acetone, ethanol in dispersion solvent
Volume ratio with acetone is (18.9-19.1):1；
Step（4）, it is spray-dried：
By step（3）Palladium solution after the dispersion obtaining uses spray dryer to be spray-dried, and obtains palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, and inlet amount is 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).
Conventionally carry out aqua regia dissolution and nitre step is caught up with in concentration, will be after palladium powder aqua regia dissolution, reheating is boiled
Boiling is done near, and then enriching hydrochloric acid carries out catching up with nitre, to not having obvious gas to escape, obtains palladium solution.
Nitre process is caught up with to can be repeated several times it is further preferred that concentrate.
It is further preferred that need heating during by palladium powder aqua regia dissolution, the mass ratio of palladium powder and chloroazotic acid is 1：3, add
Hot temperature is 100 DEG C.
It is further preferred that the nozzle diameter of described spray dryer is 0.5-3mm.
It is further preferred that step（2）In be by step（1）The palladium solution regulation obtaining is 80g/ to the concentration of palladium
L, and pH value is 1.
It is further preferred that step（3）The volume that middle dispersion solvent adds is the 5% of palladium liquor capacity.
It is further preferred that the volume ratio of ethanol and acetone is 19 in dispersion solvent:1.
It is further preferred that the described tail gas producing that is spray-dried uses alkali lye spray-absorption, absorbing liquid is by passing
The Palladium recovery technique of system carries out reclaiming.
It is further preferred that the mass concentration of described alkali lye is 40%, i.e. the mass concentration of NaOH is 40%.
Step of the present invention（2）Middle regulation palladium concentration when, use concentrate or dilution method, dilution can use water or salt
Acid.During regulation pH, the hydrochloric acid of variable concentrations and water can be used to regulate.
Present invention spray dryer to be selected is preferably Automatic Control and Non-follow control two ore control pattern, and tool
Having time set-up function, this spray dryer EAT control range is not less than 30 DEG C～300 DEG C this scopes.Preferably employ
Intelligent control system is to replace the PLC control on market, and intelligent control system is preferably formed with color LCD touch-screen parameter and shows
Show, to show the parameters such as intake air temperature, air outlet temperature, peristaltic pump rotating speed, air quantity；Use regulation and control PID thermostatic control technology,
Heated for controlling temperature precision：± 1 DEG C, the product stability so produced is higher；The evaporated water scope of this spray dryer is not little
In this scope of 1500mL/H～2000ml/h；The inlet amount of this spray dryer is adjustable, and peristaltic pump adjustable extent is not less than 50-
This scope of 2000ml/h.
Owing to spray drying device is universal standard equipment.The nozzle of equipment is the corruption that common metal cannot bear hydrochloric acid
Erosion.The nozzle material to equipment for the present invention is improved, and uses polytetrafluoroethylmaterial material thoroughly to solve what nozzle was corroded
Situation occurs, it is ensured that the quality of product.
The present invention in process of production, can realize the control of palladium bichloride product content by changing temperature and inlet amount
System, thus can meet the special requirement of client.
Compared with prior art, it has the beneficial effect that the present invention：
The present invention passes through solution concentration and adjustment and the use of acidity disperse solvent, uses spray drying device to spray simultaneously
It is dried, solve owing to technics comparing long production step will result in the problem of metal loss in current traditional handicraft, simultaneously more
Solve interpolation dispersant residue problem in the product, make product palladium bichloride be up to state standards.
Compared with traditional handicraft, it is not necessary to concentrating, crystallizing and ball milling step, the product batches obtaining is stable.Compare tradition work
Skill, loss can reduce at least 60%.
Present invention process can realize noble metal palladium bichloride compound products continuous prodution problem, with short production cycle, cost
Low, free from environmental pollution, reduce the production loss causing because of production technology length.
Present invention determine that the technological parameter that palladium bichloride is produced in batches, can prepare product in batches, product P d content >=59.8%,
Acid-soluble well, product granularity be-120 mesh, meet GB《GB/T8185-2004》The requirement of palladium bichloride crystal, properties of product
Stable, uniformity is good, and the use reaching catalyst precursor requires.
The present invention has carried out technological improvement to traditional spray drying device, to meet the need that palladium bichloride of the present invention produces
Ask.
Product of the present invention is not necessarily to ball milling, not only reduces loss, but also avoids the deliquescence of palladium bichloride, and this is for follow-up
The using effect of client gives very big lifting.Because many experiments preferably must be held in anhydrous under the conditions of carry out, if made
For the palladium bichloride of catalyst by deliquescence, then can affect experiment effect.
In terms of tail gas recycle, applicant is finally determined that by substantial amounts of experiment work employing spray-absorption method solves
Acid mist in tail gas is processed and trace palladium bichloride crystal reclaims problem, it is achieved the production of environmental protection, energy-conservation, serialization and mass.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and should not be regarded as limiting this
Bright scope.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition
Or carry out according to product description.Agents useful for same or instrument unreceipted production firm person, be and can be obtained by buying
Conventional products.
Embodiment 1
The production technology of a kind of palladium bichloride, it is characterised in that comprise the steps：
Step（1）, nitre is caught up with in aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with in concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH regulation：
By step（1）The palladium solution regulation obtaining is 79g/L to the concentration of palladium, and pH value is 0.9；
Step（3）, dispersion：
To through step（2）Adding dispersion solvent in the palladium solution of regulation, the volume that dispersion solvent adds is palladium liquor capacity
4.9%, the palladium solution after being disperseed；Described dispersion solvent is the mixture of ethanol and acetone, ethanol and third in dispersion solvent
The volume ratio of ketone is 18.9:1；
Step（4）, it is spray-dried：
By step（3）Palladium solution after the dispersion obtaining uses spray dryer to be spray-dried, and obtains palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, and inlet amount is 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).The nozzle diameter of spray dryer is 0.5mm.
Embodiment 2
The production technology of a kind of palladium bichloride, it is characterised in that comprise the steps：
Step（1）, nitre is caught up with in aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with in concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH regulation：
By step（1）The palladium solution regulation obtaining is 81g/L to the concentration of palladium, and pH value is 1.1；
Step（3）, dispersion：
To through step（2）Adding dispersion solvent in the palladium solution of regulation, the volume that dispersion solvent adds is palladium liquor capacity
5.1%, the palladium solution after being disperseed；Described dispersion solvent is the mixture of ethanol and acetone, ethanol and third in dispersion solvent
The volume ratio of ketone is 19.1:1；
Step（4）, it is spray-dried：
By step（3）Palladium solution after the dispersion obtaining uses spray dryer to be spray-dried, and obtains palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, and inlet amount is 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).The nozzle diameter of spray dryer is 3mm.
The described tail gas producing that is spray-dried uses alkali lye spray-absorption.
Embodiment 3
The production technology of a kind of palladium bichloride, it is characterised in that comprise the steps：
Step（1）, nitre is caught up with in aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step caught up with in concentration, will after palladium powder aqua regia dissolution, reheat boil to
Near dry, then enriching hydrochloric acid carries out catching up with nitre, to not having obvious gas to escape, obtains palladium solution.Concentration catches up with nitre process repeatable
Repeatedly.Needing heating during by palladium powder aqua regia dissolution, the mass ratio of palladium powder and chloroazotic acid is 1：3, heating-up temperature is 100 DEG C.
Step（2）, palladium solution concentration and pH regulation：
By step（1）The palladium solution regulation obtaining is 80g/L to the concentration of palladium, and pH value is 1；
Step（3）, dispersion：
To through step（2）Adding dispersion solvent in the palladium solution of regulation, the volume that dispersion solvent adds is the 5% of palladium liquor capacity,
Palladium solution after being disperseed；Described dispersion solvent is the mixture of ethanol and acetone, ethanol and acetone in dispersion solvent
Volume ratio is 19:1；
Step（4）, it is spray-dried：
By step（3）Palladium solution after the dispersion obtaining uses spray dryer to be spray-dried, and obtains palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, and inlet amount is 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).The nozzle diameter of spray dryer is 2mm.
Described is spray-dried the alkali lye spray-absorption that the tail gas producing uses mass concentration to be 40%.
Comparative example 1
Comparative example 1 is with the difference of embodiment 3：Step（2）It is by step（1）The palladium solution regulation obtaining to the concentration of palladium is
120g/L, remaining is all identical.
The product palladium content preparing is too high, and yield declines.
Comparative example 2
Comparative example 2 is with the difference of embodiment 3：Step（2）It is by step（1）The palladium solution regulation obtaining to the concentration of palladium is
40g/L, remaining is all identical.
The product palladium content preparing is relatively low, does not meets Standard.
Comparative example 3
Comparative example 3 is with the difference of embodiment 3：Without step（3）Dispersion steps, remaining is all identical.
There is substantial amounts of caking in the product preparing, it is desired nonetheless to ball milling, economic benefit is decreased obviously.
Comparative example 4
Comparative example 4 is with the difference of embodiment 3：The temperature being spray-dried is 110 DEG C.
The product drying preparing is incomplete, a small amount of caking phenomenon occurs, and yield declines to a great extent, and at least declines 10%.
General principle, principal character and the advantages of the present invention of the present invention have more than been shown and described.The technology of the industry
Personnel are it should be appreciated that the present invention is not restricted to the described embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (10)
1. the production technology of a palladium bichloride, it is characterised in that comprise the steps：
Step（1）, nitre is caught up with in aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with in concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH regulation：
By step（1）The palladium solution regulation obtaining is 79-81g/L to the concentration of palladium, and pH value is 0.9-1.1；
Step（3）, dispersion：
To through step（2）Adding dispersion solvent in the palladium solution of regulation, the volume that dispersion solvent adds is palladium liquor capacity
4.9-5.1%, the palladium solution after being disperseed；Described dispersion solvent is the mixture of ethanol and acetone, ethanol in dispersion solvent
Volume ratio with acetone is (18.9-19.1):1；
Step（4）, it is spray-dried：
By step（3）Palladium solution after the dispersion obtaining uses spray dryer to be spray-dried, and obtains palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, and inlet amount is 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).
2. the production technology of palladium bichloride according to claim 1, it is characterised in that conventionally carry out aqua regia dissolution
Catching up with nitre step with concentration, will reheating and boil near dry after palladium powder aqua regia dissolution, then enriching hydrochloric acid carries out catching up with nitre, extremely
Do not have obvious gas to escape, obtain palladium solution.
3. the production technology of palladium bichloride according to claim 2, it is characterised in that concentrate and catch up with nitre process can be repeated several times.
4. the production technology of palladium bichloride according to claim 2, it is characterised in that will need during palladium powder aqua regia dissolution to add
Heat, the mass ratio of palladium powder and chloroazotic acid is 1：3, heating-up temperature is 100 DEG C.
5. the production technology of palladium bichloride according to claim 1, it is characterised in that the jet hole of described spray dryer
Footpath is 0.5-3mm.
6. the production technology of palladium bichloride according to claim 1, it is characterised in that step（2）In be by step（1）Obtain
The regulation of palladium solution be 80g/L to the concentration of palladium, and pH value is 1.
7. the production technology of palladium bichloride according to claim 1, it is characterised in that step（3）Middle dispersion solvent adds
Volume is the 5% of palladium liquor capacity.
8. the production technology of palladium bichloride according to claim 1, it is characterised in that the body of ethanol and acetone in dispersion solvent
Long-pending ratio is 19:1.
9. the production technology of palladium bichloride according to claim 1, it is characterised in that described is spray-dried the tail gas producing
Use alkali lye spray-absorption.
10. the production technology of palladium bichloride according to claim 9, it is characterised in that the mass concentration of described alkali lye is
40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610763052.3A CN106430333B (en) | 2016-08-30 | 2016-08-30 | A kind of production technology of palladium bichloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610763052.3A CN106430333B (en) | 2016-08-30 | 2016-08-30 | A kind of production technology of palladium bichloride |
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| Publication Number | Publication Date |
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| CN106430333A true CN106430333A (en) | 2017-02-22 |
| CN106430333B CN106430333B (en) | 2018-03-20 |
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| CN201610763052.3A Active CN106430333B (en) | 2016-08-30 | 2016-08-30 | A kind of production technology of palladium bichloride |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1421395A (en) * | 2002-12-19 | 2003-06-04 | 国内贸易部物资再生利用研究所 | Palladium chloride producing process |
| WO2014091456A1 (en) * | 2012-12-14 | 2014-06-19 | Fer-Min-Ore (Proprietary) Limited | Process for recovering platinum group metals |
| CN104773765A (en) * | 2015-05-05 | 2015-07-15 | 昆明正江工贸有限责任公司 | Preparing method of analytically-pure palladium chloride |
-
2016
- 2016-08-30 CN CN201610763052.3A patent/CN106430333B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1421395A (en) * | 2002-12-19 | 2003-06-04 | 国内贸易部物资再生利用研究所 | Palladium chloride producing process |
| WO2014091456A1 (en) * | 2012-12-14 | 2014-06-19 | Fer-Min-Ore (Proprietary) Limited | Process for recovering platinum group metals |
| CN104773765A (en) * | 2015-05-05 | 2015-07-15 | 昆明正江工贸有限责任公司 | Preparing method of analytically-pure palladium chloride |
Non-Patent Citations (1)
| Title |
|---|
| 董树仁 等: "氯化钯的研制与应用", 《中国物资再生》 * |
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