CN109806866A - A kind of production technology of organosilicon ternary copper catalyst - Google Patents
A kind of production technology of organosilicon ternary copper catalyst Download PDFInfo
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- CN109806866A CN109806866A CN201910116090.3A CN201910116090A CN109806866A CN 109806866 A CN109806866 A CN 109806866A CN 201910116090 A CN201910116090 A CN 201910116090A CN 109806866 A CN109806866 A CN 109806866A
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Abstract
The present invention provides a kind of production technology of organosilicon ternary copper catalyst, is related to ternary copper catalyst processing technique field.The production method of the organosilicon ternary copper catalyst the following steps are included: high temperature hot melt, heat preservation hot melt, water atomization processing, vacuum dehydration, dry heat preservation, vibrosieve.The present invention overcomes the deficiencies in the prior art, using One-step production control technique, optimize production technology, make to have many advantages, such as in catalyst production process easy to operate, at low cost, and the method for the present invention produces catalyst production process green non-pollution while excellent catalytic effect, meets environmental regulations.
Description
Technical field
The present invention relates to ternary copper catalyst processing technique fields, and in particular to a kind of life of organosilicon ternary copper catalyst
Production. art.
Background technique
Organosilicon material is a major class using Si-O key as main chain, and high score of the organic group as side chain is introduced on Si atom
Sub- compound causes the chemical property of methylchlorosilane very active since it has half inorganic, half organic structure, comprehensive
The potentiality of deep processing are very big, especially hydrolysis, alcoholysis and correlated response, therefore have many excellent performances and special function
Energy.Organic silicon monomer is the base stock for manufacturing organosilicon material, and the dimethyl dichloro wherein obtained by direct synthesis technique
Silane accounts for 90% or more of the total dosage of organic silicon monomer.Dimethyldichlorosilane is the maximum monomer of practical value, by its system
The most important intermediate of octamethylcy-clotetrasiloxane series silicone industry obtained, purposes are extremely extensive.It sums up, methyl chloride
Silane deep processing mainly has: the four major class product such as silicon rubber, silicone resin, silane coupling agent and silicone oil.Due to methylchlorosilane depth
Converted products has good weatherability variation, anti-aging, electrical insulation properties and good biocompatibility and performance of surging by force etc. excellent
Performance is widely used in automobile manufacture, petrochemical industry, rubber industry, numerous industries such as polyurethane industrial, methylchlorosilane derivative
Product is considered as general effective and durable industrial materials.
Due to the extensive use of ternary copper catalyst, China is also relatively more active to the research of cuprous oxide in recent years, oxidation
Cuprous preparation method can about be divided into following three kinds: sintering process, electrolysis method and wet reducing method.
Sintering process is also known as dry method, and this method is to be pre-mixed solid copper powder with cupric oxide powder, is re-fed into incinerator
Interior heating reaction.Following reaction occurs therebetween:
CuO+Cu=Cu2O
The method is easy, and cuprous oxide powder degree of oxidation obtained is higher, and condition is easy to control, is suitble to industry raw
It produces.
Make anode in the solution containing copper ion with metallic copper to be electrolysed, it is sub- that the higher oxidation of purity can be obtained on cathode
Copper powders.In the NaCl alkaline aqueous solution containing NaOH when electrolytic metal Cu, cathode and anode will occur as follows respectively
Electrode reaction:
Anode: Cu+Cl-=(CuCl-)
Cathode: 2H2O+2e=H2+2OH-
Electrode net reaction: 2Cu+H2O=H2+Cu2O
In terms of Reactive Mechanism of Electrode, cuprous oxide powder be by anode copper dissolution, made of hydrolytic precipitation reaction occurs,
OH needed for reacting-It is the OH generated by cathodic region-It is obtained by diffusion, migration.In terms of net reaction, electrolytic process is anode
The dissolution of copper and the consumption process of water are generated without other side reactions.The Cu prepared with the method2O powder takes on a red color, dispersion performance
It is good, it is suitable for ship bottom antifouling paint.But this method power consumption is high, low output, thus its development is subject to certain restrictions.
In recent years, since the obtained cuprous oxide powder partial size of wet-chemical reduction method is small, with high purity, dispersion performance is good.
It gets more and more attention, the preparation method that oneself gropes now can be divided into sulphite, hydration takes off, warp according to the difference of reducing agent
Amine, rongalite, copper powder, zinc powder, hydro-thermal hydrogenating reduction method etc. are several, are all that the copper ion reduction in solution is obtained oxidation Asia
Copper.Wet-chemical reduction method prepares cuprous oxide and is still limited to laboratory research at present at home, be converted into it is industrial compared with
Less and the cuprous oxide product prepared that there are the unstable impurity contents of performance compared with external product is higher, form and aspect are unstable,
The disadvantages of raw material availability is low, energy consumption is relatively high.Due to the difference of process conditions, obtained particle size is also different, even
Composition is also different.Even method of the same race, obtained particle size is also different.So receiving very big limit in industrial production
System.
But either sintering process, electrolysis method or wet reducing method must all carry out ball-milling technology ball to be applied to production
Mill, could improve its catalytic performance, reach catalysis purpose.Complex process is cumbersome, at high cost.
Summary of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of production technology of organosilicon ternary copper catalyst, using a step
Method production control technique, optimize production technology, make to have many advantages, such as in catalyst production process it is easy to operate, at low cost,
And the method for the present invention produces catalyst production process green non-pollution while excellent catalytic effect, meets environmental regulations.
In order to achieve the above object, technical solution of the present invention is achieved by the following technical programs:
A kind of production technology of organosilicon ternary copper catalyst, the production method of the catalyst the following steps are included:
(1) will be melted in fine copper addition middle frequency furnace using 1200-1500 DEG C of high-temperature heat is molten into raw material all
Copper water, and the condition of high temperature melting is to contact heat with air to melt；
(2) after above-mentioned copper water heat preservation hot being melted a period of time, the copper water stream of melting is hit using 60-100MPa high pressure water flow
D50 is broken into the copper powder of 13um, it is spare；
(3) above-mentioned copper powder is dehydrated under vacuum environment, 150-380 DEG C of high temperature drying is carried out in drying oven
Afterwards, continue to keep the temperature continued oxidation for a period of time, it is spare to obtain ternary copper powder；
(4) above-mentioned ternary copper powder is subjected to the Ternary copper that vibration filters out required partial size, obtains organosilicon ternary of the present invention
Copper catalyst.
Preferably, the ratio of the ternary component of the organosilicon ternary copper catalyst are as follows: metallic copper 10-40%, oxidation are sub-
Copper 25-80%, copper oxide 15-65%.
Preferably, the temperature that electric furnace high temperature heat is melted in the step (1) is 1250-1350 DEG C.
Preferably, the time that heat preservation hot is melted in the step (2) is 40-50min, and the pressure of high pressure water flow is 80Mpa.
Preferably, drying temperature is 250-300 DEG C in the step (3), and the time for keeping the temperature continued oxidation is 1-2h.
Preferably, Ternary copper is sieved using -625 mesh of 1250 mesh in the step (4).
The present invention provides a kind of production technology of organosilicon ternary copper catalyst, and advantage is compared with prior art:
(1) present invention under the conditions of oxygen-containing using high temperature hot melt is carried out by fine copper, when fine copper is melted in intermediate frequency furnace high temperature
When, it is contacted with oxygen, generate cuprous oxide: 4Cu+O2=2Cu2O cuprous oxide generated is dissolved in copper melts immediately, oxidation
The cuprous solubility in copper solution, increases with increasing temperature, when being greater than a certain temperature, Cu2O contains temperature in melt
When amount is more than 12.4% or more, melt is classified into two layers, is the superfluous cuprous oxide being precipitated in the melt upper surface of saturation Cu2O.
It is dissolved in the cuprous oxide in copper water as the extension production quantity of oxidization time can be more and more, as shown in the table:
The solubility of cuprous oxide:
It is cheaper and easy to operate to melt cost compared to traditional nitrogen protection heat, products obtained therefrom is conducive to later period system
It is standby.
(2) present invention uses water atomization to melt molten metal to heat and carries out powder processed, and is carried out using 60-100MPa high pressure water flow
Processing, can effectively obtain the metal powder of required partial size, reach the operation purpose of high-efficiency environment friendly.
(3) present invention is handled by the way of high temperature drying after vacuum dehydration after water atomization prepares copper powder, wherein copper powder
Part copper powder is set to be oxidized to copper oxide during drying.Powder after drying is then by copper oxide, cuprous oxide, copper three
The Ternary copper of composition prepares ternary copper powder, needs not move through ball-milling technology ball milling, this production method is easy to operate high-efficient, is suitble to push away
It is wide to use.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below with reference to the embodiment of the present invention pair
Technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is a part of the invention
Embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making wound
Every other embodiment obtained under the premise of the property made labour, shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of production technology of organosilicon ternary copper catalyst, the production method of the catalyst the following steps are included:
(1) will be melted in fine copper addition middle frequency furnace using 1250 DEG C of high-temperature heat makes raw material all be molten into copper water,
And the condition of high temperature melting is to contact heat with air to melt；
(2) after above-mentioned copper water heat preservation hot being melted 40-50min, the copper water stream of melting is smashed into using 60MPa high pressure water flow
D50 13um copper powder, it is spare；
(3) above-mentioned copper powder is dehydrated under vacuum environment, after carrying out 200 DEG C of high temperature dryings in drying oven, after
Continue insurance warm continued oxidation 1-2h, and it is spare to obtain ternary copper powder；
(4) above-mentioned ternary copper powder is subjected to the Ternary copper that vibration filters out required partial size using -625 mesh of 1250 mesh, obtained
To organosilicon ternary copper catalyst of the present invention.
Wherein, the ratio of the ternary component of the organosilicon ternary copper catalyst are as follows: metallic copper 10-40%, cuprous oxide
25-80%, copper oxide 15-65%.
Embodiment 2:
A kind of production technology of organosilicon ternary copper catalyst, the production method of the catalyst the following steps are included:
(1) will be melted in fine copper addition middle frequency furnace using 1300 DEG C of high-temperature heat makes raw material all be molten into copper water,
And the condition of high temperature melting is to contact heat with air to melt；
(2) after above-mentioned copper water heat preservation hot being melted 40-50min, the copper water stream of melting is smashed into using 80MPa high pressure water flow
D50 13um copper powder, it is spare；
(3) above-mentioned copper powder is dehydrated under vacuum environment, after carrying out 250 DEG C of high temperature dryings in drying oven, after
Continue insurance warm continued oxidation 1-2h, and it is spare to obtain ternary copper powder；
(4) above-mentioned ternary copper powder is subjected to the Ternary copper that vibration filters out required partial size using -625 mesh of 1250 mesh, obtained
To organosilicon ternary copper catalyst of the present invention.
Wherein, the ratio of the ternary component of the organosilicon ternary copper catalyst are as follows: metallic copper 10-40%, cuprous oxide
25-80%, copper oxide 15-65%.
Embodiment 3:
A kind of production technology of organosilicon ternary copper catalyst, the production method of the catalyst the following steps are included:
(1) will be melted in fine copper addition middle frequency furnace using 1350 DEG C of high-temperature heat makes raw material all be molten into copper water,
And the condition of high temperature melting is to contact heat with air to melt；
(2) after above-mentioned copper water heat preservation hot being melted 40-50min, the copper water stream of melting is smashed using 100MPa high pressure water flow
At D50 13um copper powder, it is spare；
(3) above-mentioned copper powder is dehydrated under vacuum environment, after carrying out 300 DEG C of high temperature dryings in drying oven, after
Continue insurance warm continued oxidation 1-2h, and it is spare to obtain ternary copper powder；
(4) above-mentioned ternary copper powder is subjected to the Ternary copper that vibration filters out required partial size using -625 mesh of 1250 mesh, obtained
To organosilicon ternary copper catalyst of the present invention.
Wherein, the ratio of the ternary component of the organosilicon ternary copper catalyst are as follows: metallic copper 10-40%, cuprous oxide
25-80%, copper oxide 15-65%.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of production technology of organosilicon ternary copper catalyst, which is characterized in that the production method of the catalyst include with
Lower step:
(1) will be melted in fine copper addition middle frequency furnace using 1200-1500 DEG C of high-temperature heat makes raw material all be molten into copper water,
And the condition of high temperature melting is to contact heat with air to melt；
(2) after above-mentioned copper water heat preservation hot being melted a period of time, the copper water stream of melting is smashed into using 60-100MPa high pressure water flow
D50 13um copper powder, it is spare；
(3) above-mentioned copper powder is dehydrated under vacuum environment, after carrying out 150-380 DEG C of high temperature drying in drying oven, after
Warm continued oxidation continue insurance for a period of time, it is spare to obtain ternary copper powder；
(4) above-mentioned ternary copper powder is subjected to the Ternary copper that vibration filters out required partial size, obtains organosilicon Ternary copper of the present invention and urges
Agent.
2. a kind of production technology of organosilicon ternary copper catalyst according to claim 1, which is characterized in that described organic
The ratio of the ternary component of silicon ternary copper catalyst are as follows: metallic copper 10-40%, cuprous oxide 25-80%, copper oxide 15-65%.
3. a kind of production technology of organosilicon ternary copper catalyst according to claim 1, it is characterised in that: the step
(1) temperature that electric furnace high temperature heat is melted in is 1250-1350 DEG C.
4. a kind of production technology of organosilicon ternary copper catalyst according to claim 1, it is characterised in that: the step
(2) time that heat preservation hot is melted in is 40-50min, and the pressure of high pressure water flow is 80Mpa.
5. a kind of production technology of organosilicon ternary copper catalyst according to claim 1, it is characterised in that: the step
(3) drying temperature is 250-300 DEG C in, and the time for keeping the temperature continued oxidation is 1-2h.
6. a kind of production technology of organosilicon ternary copper catalyst according to claim 1, it is characterised in that: the step
(4) Ternary copper is sieved using -625 mesh of 1250 mesh in.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209978A (en) * | 2021-05-07 | 2021-08-06 | 江苏库博德金属科技有限公司 | Organic silicon high-activity ternary copper catalyst and preparation method thereof |
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| CN1156640A (en) * | 1995-12-01 | 1997-08-13 | 拜尔公司 | Copper-based catalysts, processes for their production and their use and process for production of alkyl halosilanes |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113209978A (en) * | 2021-05-07 | 2021-08-06 | 江苏库博德金属科技有限公司 | Organic silicon high-activity ternary copper catalyst and preparation method thereof |
| CN113209978B (en) * | 2021-05-07 | 2023-08-29 | 江苏库博德金属科技有限公司 | Organosilicon high-activity ternary copper catalyst and preparation method thereof |
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Application publication date: 20190528 |