CN104743535A - Production method of copper pyrophosphate - Google Patents
Production method of copper pyrophosphate Download PDFInfo
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- CN104743535A CN104743535A CN201510136154.8A CN201510136154A CN104743535A CN 104743535 A CN104743535 A CN 104743535A CN 201510136154 A CN201510136154 A CN 201510136154A CN 104743535 A CN104743535 A CN 104743535A
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- pyrophosphate
- cupric
- cupric pyrophosphate
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Abstract
The invention provides a production method of copper pyrophosphate. Copper pyrophosphate is generated by virtue of reaction of copper nitrate and sodium pyrophosphate, wherein the pH is controlled at 3.5-4 in the reaction process of copper nitrate and sodium pyrophosphate, and the pH is controlled at 4.5-5.5 when precipitates are no long generated as the reaction approaches the finish point. The obtained copper pyrophosphate is high in purity and the content is greater than 34.0% (based on the content of copper). Insoluble double salts of copper pyrophosphate in copper pyrophosphate are extremely less and are less than 0.1%, so that the copper pyrophosphate is relatively good in effect during electroplating.
Description
Technical field
The present invention relates to a kind of production method of cupric pyrophosphate, be specifically related to a kind of production method of electroplating with cupric pyrophosphate.
Background technology
Cupric pyrophosphate is a kind of light blue crystal, and usual molecule is Cu
2p
2o
73H
2o, loses crystal water and becomes blue powder.Be dissolved in acid, water insoluble.Can form water-soluble complex salt with potassium pyrophosphate, have stronger complex ability to metal ion, the electroconductibility of solution is high, and during for electroplating, the current efficiency of negative electrode and anode is close to 100%.Therefore it is mainly used in cyanideless electro-plating and anti-carburization coating, also can be used for configuring phosphate pigment.Meanwhile, cupric pyrophosphate also has other composite salt, as: Na
32cu
14(P
2o
7)
1513H
2o; Na
4cu
8(P
2o
7)
517H
2o, the two is light blue insolubles.
Existing technology carries out replacement(metathesis)reaction with soluble copper salt and soluble pyrophosphate, generates cupric pyrophosphate, and be generally dichloride copper or copper sulfate and trisodium phosphate, its shortcoming is that product easily forms insoluble mixing salt.
Summary of the invention
For solving the Problems existing of above-mentioned prior art, the object of the present invention is to provide a kind of insoluble mixing salt low, the plating cupric pyrophosphate that purity is high.
The object of the invention is to be realized by following measures:
A production method for cupric pyrophosphate, adopts cupric nitrate and trisodium phosphate react and generates cupric pyrophosphate, and in cupric nitrate and trisodium phosphate reaction process, pH controls to be 3.5 ~ 4, reacts no longer to produce close to terminal that to precipitate pH control be afterwards 4.5 ~ 5.5.
The production method of above-mentioned cupric pyrophosphate, also comprises cupric pyrophosphate wet product dry at reduced pressure conditions, obtains finished product cupric pyrophosphate.Preferably, to be employing condition be drying under reduced pressure: pressure is 0.01MPa ~ 0.02MPa, and temperature is 70 ~ 100 DEG C, dry 4 ~ 6h.
Above-mentioned cupric nitrate and trisodium phosphate reaction comprise the following steps: in reactor, add water of a certain amount of end, be heated to 70-90 DEG C, under agitation condition, the flow velocity of mass concentration 15% sodium pyrophosphate solution and mass concentration 20% copper nitrate solution is added in reactor with 1200L/h and 500L/h flow velocity respectively, keep temperature of reaction at 70 DEG C ~ 80 DEG C, in reaction process, pH is 3.5 ~ 4, react and (no longer include precipitation to produce) close to after terminal, be adjusted to pH=4.5 ~ 5.5, the reaction times controls at 1h ~ 2h.After having reacted, by reaction solution centrifugation, and use water centrifuge washing, obtain cupric pyrophosphate wet product, cupric pyrophosphate wet product is dry at reduced pressure conditions, obtain finished product cupric pyrophosphate.
Above-mentioned cupric nitrate is that copper and nitric acid reaction generate.
Beneficial effect
1, the cupric pyrophosphate purity of gained of the present invention is high, and content is greater than 34.0% (with copper content meter).In cupric pyrophosphate, insoluble cupric pyrophosphate double salt is few, is less than 0.1%, makes cupric pyrophosphate better effects if when electroplating.
2, present invention process process is simple, and mild condition is easy to control, and raw material sources are convenient.For actual industrial production.
Embodiment
Be described in further detail the specific embodiment of the present invention below in conjunction with embodiment, but invention is not limited to present embodiment, any improvement or alternative on the present embodiment essence spirit, still belongs to the claims in the present invention scope required for protection.
Embodiment 1
A production method for cupric pyrophosphate, comprises the following steps:
(1) get 35kg copper and nitric acid reaction, produce copper nitrate solution, pH=4, concentration is 20%;
(2) solution that 100kg trisodium phosphate is made into 15% is got;
(3) in reactor, quantitative end water is added, be heated to 80 DEG C, under agitation condition, add in reactor with certain flow rate by sodium pyrophosphate solution and copper nitrate solution, the flow velocity of sodium pyrophosphate solution and copper nitrate solution is 1200L/h and 500L/h respectively simultaneously, keeps temperature of reaction at 70 DEG C, keep reaction process pH 3.5, reaction is close to after terminal, and be adjusted to pH=4.5, the reaction times controls at 1.5h.After having reacted, by reaction solution centrifugation, and use water centrifuge washing, obtain cupric pyrophosphate wet product.
(4) cupric pyrophosphate wet product is dry at reduced pressure conditions, adopt pressure 0.02MPa, temperature is 100 DEG C, time 5h.Obtain finished product cupric pyrophosphate.
After testing, the insolubles of gained cupric pyrophosphate in potassium pyrophosphate solution is 0.06%, content 34.2% (with copper content meter), iron level 0.007%, and arsenic content is less than 0.0003%, granularity 100 μm.
Embodiment 2
A production method for cupric pyrophosphate, comprises the following steps:
(1) get 35kg copper and nitric acid reaction, produce copper nitrate solution, pH=4, concentration is 20%;
(2) solution that 100kg trisodium phosphate is made into 15% is got;
(3) in reactor, quantitative end water is added, be heated to 90 DEG C, under agitation condition, sodium pyrophosphate solution and copper nitrate solution add in reactor with certain flow rate simultaneously, the flow velocity of sodium pyrophosphate solution and copper nitrate solution is 1200L/h and 500L/h respectively, keeps temperature of reaction at 80 DEG C, keeps reaction process pH 4, reaction, close to after terminal, is adjusted to pH=5.Reaction times controls at 1h ~ 2h.After having reacted, by reaction solution centrifugation, and use water centrifuge washing, obtain cupric pyrophosphate wet product.
(4) cupric pyrophosphate wet product is dry at reduced pressure conditions, adopt pressure 0.01MPa, temperature is 90 DEG C, time 6h.Obtain finished product cupric pyrophosphate.
After testing, the insolubles of gained cupric pyrophosphate in potassium pyrophosphate solution is 0.05%, content 34.2% (with copper content meter), iron level 0.005%, and arsenic content is less than 0.0003%, granularity 102 μm.
Embodiment 3
A production method for cupric pyrophosphate, comprises the following steps:
(1) get 35kg copper and nitric acid reaction, produce copper nitrate solution, pH=4, concentration is 20%;
(2) solution that 100kg trisodium phosphate is made into 15% is got;
(3) in reactor, quantitative end liquid is added, be heated to 90 DEG C, under agitation condition, sodium pyrophosphate solution and copper nitrate solution add in reactor with certain flow rate simultaneously, the flow velocity of sodium pyrophosphate solution and copper nitrate solution is 1200L/h and 500L/h respectively, keeps temperature of reaction at 75 DEG C, keeps reaction process pH 3.5, reaction, close to after terminal, is adjusted to pH5.5.Reaction times controls at 2h.After having reacted, by reaction solution centrifugation, and use water centrifuge washing, obtain cupric pyrophosphate wet product.
(4) cupric pyrophosphate wet product is dry at reduced pressure conditions, adopt pressure 0.01MPa, temperature is 80 DEG C, time 4h.Obtain finished product cupric pyrophosphate.
After testing, the insolubles of gained cupric pyrophosphate in potassium pyrophosphate solution is 0.06%, content 34.3% (with copper content meter), iron level 0.006%, and arsenic content is less than 0.0003%, granularity 98 μm.
Claims (5)
1. a production method for cupric pyrophosphate, adopts cupric nitrate and trisodium phosphate react and generates cupric pyrophosphate, and in cupric nitrate and trisodium phosphate reaction process, pH controls to be 3.5 ~ 4, reacts no longer to produce close to terminal that to precipitate pH control be afterwards 4.5 ~ 5.5.
2. the production method of cupric pyrophosphate as claimed in claim 1, also comprises cupric pyrophosphate wet product dry at reduced pressure conditions, obtains finished product cupric pyrophosphate.
3. the production method of cupric pyrophosphate as claimed in claim 1 or 2, drying under reduced pressure condition is: pressure is 0.01MPa ~ 0.02MPa, and temperature is 70 ~ 100 DEG C, dry 4 ~ 6h.
4. the production method of cupric pyrophosphate as claimed in claim 1, comprise the following steps: in reactor, add water of a certain amount of end, be heated to 70-90 DEG C, under agitation condition, the flow velocity of mass concentration 15% sodium pyrophosphate solution and mass concentration 20% copper nitrate solution is added in reactor with 1200L/h and 500L/h flow velocity respectively, keep temperature of reaction at 70 DEG C ~ 80 DEG C, in reaction process, pH is 3.5 ~ 4, react after no longer including precipitation generation close to terminal, be adjusted to pH=4.5 ~ 5.5, the reaction times controls at 1h ~ 2h; Then by reaction solution centrifugation, and use water centrifuge washing, obtain cupric pyrophosphate wet product, be 0.01MPa ~ 0.02MPa by cupric pyrophosphate wet product at pressure, temperature is under 70 ~ 100 DEG C of conditions, and dry 4 ~ 6h, obtains finished product cupric pyrophosphate.
5. the production method of cupric pyrophosphate as claimed in claim 1, described cupric nitrate is that copper and nitric acid reaction generate.
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|---|---|---|---|
| CN201510136154.8A CN104743535A (en) | 2015-03-26 | 2015-03-26 | Production method of copper pyrophosphate |
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|---|---|---|---|
| CN201510136154.8A CN104743535A (en) | 2015-03-26 | 2015-03-26 | Production method of copper pyrophosphate |
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| CN104743535A true CN104743535A (en) | 2015-07-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108883945A (en) * | 2016-03-29 | 2018-11-23 | 富圣宝利通股份有限公司 | Whiteness of absorption near infrared ray and preparation method thereof |
-
2015
- 2015-03-26 CN CN201510136154.8A patent/CN104743535A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108883945A (en) * | 2016-03-29 | 2018-11-23 | 富圣宝利通股份有限公司 | Whiteness of absorption near infrared ray and preparation method thereof |
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Application publication date: 20150701 |
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