CN106430333B - A kind of production technology of palladium bichloride - Google Patents
A kind of production technology of palladium bichloride Download PDFInfo
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- CN106430333B CN106430333B CN201610763052.3A CN201610763052A CN106430333B CN 106430333 B CN106430333 B CN 106430333B CN 201610763052 A CN201610763052 A CN 201610763052A CN 106430333 B CN106430333 B CN 106430333B
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Abstract
The present invention relates to a kind of production technology of palladium bichloride, belong to chemical technology field.The technique includes aqua regia dissolution and nitre, palladium solution concentration and pH regulations, scattered and four big steps of spray drying are caught up with concentration.The present invention is by the adjustment of solution concentration and acidity and uses dispersion solvent, it is spray-dried simultaneously using spray drying device, solve the problems, such as in current traditional handicraft because technics comparing long production step will result in metal loss more, solve the residue problem of addition dispersant in the product simultaneously, product palladium bichloride is up to state standards.Compared with traditional handicraft, without concentrating, crystallizing and ball milling step, obtained product batches are stable.Compared to traditional handicraft, loss can reduce at least 60%.Pd content >=59.8% in the product of preparation, acid-soluble good, product granularity is 120 mesh, meets national standard《GB/T8185‑2004》Requirement.
Description
Technical field
The invention belongs to metal in Chemical Manufacture to sort technical field, and in particular to a kind of production technology of palladium bichloride.
Background technology
With the continuous development of China's manufacture level, to selectivity possessed by palladium catalyst, stability, catalytic activity
It is required that also improve constantly.The palladium compound product for being commonly used as presoma at present is mainly palladium bichloride.The 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 dosage of current domestic palladium catalyst converts into palladium meter and reached 30 tons/year.Work
Industry palladium catalyst can be divided into two classes, first, homogeneous catalyst is types of functionality palladium compound, Typical Representative such as palladium；Two
It is supported catalyst, such as palladium charcoal, palladium aluminum oxide, auto-exhaust catalyst are one of them（The compound oxidizings such as palladium rhodium
Alumina supporter catalyst）, it is other to also have disproportionated rosin palladium carbon catalyst, the industrial palladium aluminium oxide catalyst of hydrogen peroxide etc..It is state
Interior most commonly used palladium catalyst presoma.The traditional processing technology of domestic palladium bichloride is at present：
。
Due to will result in the loss of metal technics comparing long production step in traditional processing technology, while also making more
Unstable into product batches, cost is high.In addition, in the industrial production, the chlorination obtained in traditional processing technology after condensing crystallizing
Palladium product is mostly bulk, it is necessary to by ball milling, can just obtain powder.
Although powder just can be obtained to crystalline product drying disclosed in present many patents, it is substantially all in these patents
It is the miniature meeting small-scale test in experiment, and it is really not so in the industrial production.In the industrial production, but dry after product
It is substantially block, it is necessary to carry out ball milling, can just obtain powder-product.
Present patent application is directed to above-mentioned condition, carries out the production Technology research and development of palladium bichloride, can be realized continuously with obtaining
Metaplasia is produced, and product batches are stable, is reduced production craft step, is reduced the production and processing technology of metal loss, be palladium catalyst row
Industry provide it is more reliable, using more convenient persursor material, extension rare precious metal industry industrial chain, fill a hole in the market,
Promote industry development.
The content of the invention
For above mentioned problem existing for current palladium bichloride, a kind of technique of present invention offer is simple, with short production cycle, cost
It is low, free from environmental pollution, acid-soluble good, the production technology of the stable palladium bichloride of palladium content.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of production technology of palladium bichloride, it is characterised in that comprise the following steps：
Step（1）, nitre is caught up with aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH are adjusted：
By step（1）It is 79-81g/L that obtained palladium solution, which is adjusted to the concentration of palladium, and pH value is 0.9-1.1；
Step（3）, disperse：
To through step（2）Dispersion solvent is added 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, second in dispersion solvent
The volume ratio of alcohol and acetone is (18.9-19.1):1；
Step（4）, spray drying：
By step（3）Obtain it is scattered after palladium solution be spray-dried using spray dryer, obtain palladium bichloride powder
End；The temperature of spray drying is 160-200 DEG C, inlet amount 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 concentration, i.e., by 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 obvious gas effusion, obtains palladium solution.
It is further preferred that concentration flooding process can be repeated several times.
It is further preferred that by palladium powder with aqua regia dissolution when need to heat, 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）It is 80g/ that obtained palladium solution, which is adjusted 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 tail gas caused by described spray drying uses alkali lye spray-absorption, absorbing liquid passes through biography
The Palladium recovery technique of system is reclaimed.
It is further preferred that the mass concentration of described alkali lye is 40%, i.e., the mass concentration of sodium hydroxide is 40%.
Step of the present invention（2）During the concentration of middle regulation palladium, using the method for concentration or dilution, dilution can use water or salt
Acid.When adjusting pH, it can be adjusted using the hydrochloric acid and water of various concentrations.
Present invention spray dryer to be selected is preferably Automatic Control and control double control pattern manually, and is had
Having time set-up function, the spray dryer EAT control range are not less than 30 DEG C~300 DEG C this scopes.It is preferred that use
To substitute the PLC of in the market to control, intelligent control system is preferably formed with color LCD touch-screen parameter and shown intelligent control system
Show, to show the parameters such as intake air temperature, air outlet temperature, wriggling revolution speed, air quantity；Using regulation and control PID thermostatic control technologies,
Heated for controlling temperature precision：± 1 DEG C, the product stability so produced is stronger；The evaporated water scope of the spray dryer is not small
In this scope of 1500mL/H~2000ml/h；The inlet amount of the spray dryer is adjustable, and peristaltic pump adjustable extent is not less than 50-
This scope of 2000ml/h.
Because spray drying device is universal standard equipment.The nozzle of equipment is the corruption that common metal can not bear hydrochloric acid
Erosion.The present invention is improved the nozzle material of equipment, thoroughly solves what nozzle was corroded using polytetrafluoroethylmaterial material
Situation occurs, and ensure 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, can thus meet the special requirement of client.
Compared with prior art, its advantage is the present invention：
The present invention is carried out by the adjustment of solution concentration and acidity and using dispersion solvent using spray drying device
Spray drying, solve the problems, such as because technics comparing long production step will result in metal loss more in current traditional handicraft,
Solve the residue problem of addition dispersant in the product simultaneously, product palladium bichloride is up to state standards.
Compared with traditional handicraft, without concentrating, crystallizing and ball milling step, obtained product batches are stable.Compared to traditional work
Skill, loss can reduce at least 60%.
Present invention process can realize noble metal palladium bichloride compound products continuous production problem, with short production cycle, cost
It is low, free from environmental pollution, reduce because production technology is long and caused by produce loss.
Present invention determine that the technological parameter of palladium bichloride batch production, can prepare product in batches, product Pd content >=59.8%,
Acid-soluble good, product granularity is -120 mesh, meets national standard《GB/T8185-2004》The requirement of palladium bichloride crystal, properties of product
Stable, uniformity is good, reaches the requirement of catalyst precursor.
The present invention has carried out technological improvement to traditional spray drying device, to meet the need of palladium bichloride production of the present invention
Ask.
Product of the present invention not only reduces loss without ball milling, and also avoid the deliquescence of palladium bichloride, and this is for follow-up
The using effect of client gives very big lifting.Because it is many experiment preferably must be held in it is anhydrous under the conditions of carry out, if make
For catalyst palladium bichloride by deliquescence, then can influence experiment effect.
In terms of tail gas recycle, applicant finally determines solve using spray-absorption method by substantial amounts of experiment work
Acid mist processing and micro palladium bichloride crystal recovery problem in tail gas, realize environmental protection, energy-conservation, serialization and the production of mass.
Embodiment
With reference to 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 it should not be regarded as limiting this hair
Bright scope.In the examples where no specific technique or condition is specified, according to the technology or condition described by document in the art
Or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument, it is that can be obtained by buying
Conventional products.
Embodiment 1
A kind of production technology of palladium bichloride, it is characterised in that comprise the following steps：
Step（1）, nitre is caught up with aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH are adjusted：
By step（1）It is 79g/L that obtained palladium solution, which is adjusted to the concentration of palladium, and pH value is 0.9；
Step（3）, disperse：
To through step（2）Dispersion solvent is added 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, in dispersion solvent ethanol and
The volume ratio of acetone is 18.9:1；
Step（4）, spray drying：
By step（3）Obtain it is scattered after palladium solution be spray-dried using spray dryer, obtain palladium bichloride powder
End；The temperature of spray drying is 160-200 DEG C, inlet amount 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
A kind of production technology of palladium bichloride, it is characterised in that comprise the following steps：
Step（1）, nitre is caught up with aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH are adjusted：
By step（1）It is 81g/L that obtained palladium solution, which is adjusted to the concentration of palladium, and pH value is 1.1；
Step（3）, disperse：
To through step（2）Dispersion solvent is added 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, in dispersion solvent ethanol and
The volume ratio of acetone is 19.1:1；
Step（4）, spray drying：
By step（3）Obtain it is scattered after palladium solution be spray-dried using spray dryer, obtain palladium bichloride powder
End；The temperature of spray drying is 160-200 DEG C, inlet amount 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).The nozzle diameter of spray dryer is 3mm.
Tail gas caused by described spray drying uses alkali lye spray-absorption.
Embodiment 3
A kind of production technology of palladium bichloride, it is characterised in that comprise the following steps：
Step（1）, nitre is caught up with aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with concentration, i.e., by 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 obvious gas effusion, obtains palladium solution.Concentrating flooding process can
Repeatedly.Need to heat during by palladium powder with 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 are adjusted：
By step（1）It is 80g/L that obtained palladium solution, which is adjusted to the concentration of palladium, and pH value is 1；
Step（3）, disperse：
To through step（2）Dispersion solvent is added in the palladium solution of regulation, the volume that dispersion solvent adds is palladium liquor capacity
5%, 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；
Step（4）, spray drying：
By step（3）Obtain it is scattered after palladium solution be spray-dried using spray dryer, obtain palladium bichloride powder
End；The temperature of spray drying is 160-200 DEG C, inlet amount 1000-1500mL/h；
The material of the nozzle of described spray dryer is polytetrafluoroethylene (PTFE).The nozzle diameter of spray dryer is 2mm.
Tail gas caused by described spray drying use mass concentration for 40% alkali lye spray-absorption.
Comparative example 1
The difference of comparative example 1 and embodiment 3 is：Step（2）It is by step（1）Obtained palladium solution adjusts dense to palladium
Spend for 120g/L, remaining is all identical.
Obtained product palladium content is too high, and yield declines.
Comparative example 2
The difference of comparative example 2 and embodiment 3 is：Step（2）It is by step（1）Obtained palladium solution adjusts dense to palladium
Spend for 40g/L, remaining is all identical.
Obtained product palladium content is relatively low, does not meet Standard.
Comparative example 3
The difference of comparative example 3 and embodiment 3 is：Without step（3）Dispersion steps, remaining is all identical.
There is substantial amounts of caking in obtained product, it is desired nonetheless to which ball milling, economic benefit are decreased obviously.
Comparative example 4
The difference of comparative example 4 and embodiment 3 is：The temperature of spray drying is 110 DEG C.
Obtained product drying 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 has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above 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, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of production technology of palladium bichloride, it is characterised in that comprise the following steps：
Step（1）, nitre is caught up with aqua regia dissolution and concentration：
Conventionally carry out aqua regia dissolution and nitre step is caught up with concentration, obtain palladium solution；
Step（2）, palladium solution concentration and pH are adjusted：
By step（1）It is 79-81g/L that obtained palladium solution, which is adjusted to the concentration of palladium, and pH value is 0.9-1.1；
Step（3）, disperse：
To through step（2）Dispersion solvent is added 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）, spray drying：
By step（3）Obtain it is scattered after palladium solution be spray-dried using spray dryer, obtain palladium bichloride powder；Spray
The temperature that mist is dried is 160-200 DEG C, inlet amount 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
Nitre step is caught up with concentration, i.e., by after palladium powder aqua regia dissolution, reheating is boiled to closely doing, and then enriching hydrochloric acid carries out catching up with nitre, extremely
There is no obvious gas to escape, obtain palladium solution.
3. the production technology of palladium bichloride according to claim 2, it is characterised in that concentration flooding process can be repeated several times.
4. the production technology of palladium bichloride according to claim 2, it is characterised in that will need to add during palladium powder aqua regia dissolution
The mass ratio of heat, 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
Palladium solution to adjust to the concentration of palladium be 80g/L, and pH value is 1.
7. the production technology of palladium bichloride according to claim 1, it is characterised in that step（3）What middle dispersion solvent added
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
Product is than being 19:1.
9. the production technology of palladium bichloride according to claim 1, it is characterised in that tail gas caused by described spray drying
Using 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%。
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| CN201610763052.3A CN106430333B (en) | 2016-08-30 | 2016-08-30 | A kind of production technology of palladium bichloride |
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| CN201610763052.3A CN106430333B (en) | 2016-08-30 | 2016-08-30 | A kind of production technology of palladium bichloride |
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| CN106430333B true CN106430333B (en) | 2018-03-20 |
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| CN1151972C (en) * | 2002-12-19 | 2004-06-02 | 国内贸易部物资再生利用研究所 | Palladium chloride producing process |
| AP2015008588A0 (en) * | 2012-12-14 | 2015-07-31 | Fer Min Ore Proprietary Ltd | 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 |
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