CN117586508A - Single-component platinum catalyst and preparation method thereof - Google Patents
Single-component platinum catalyst and preparation method thereof Download PDFInfo
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- CN117586508A CN117586508A CN202311659409.XA CN202311659409A CN117586508A CN 117586508 A CN117586508 A CN 117586508A CN 202311659409 A CN202311659409 A CN 202311659409A CN 117586508 A CN117586508 A CN 117586508A
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000003054 catalyst Substances 0.000 title claims abstract description 70
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims abstract description 95
- DVMZCYSFPFUKKE-UHFFFAOYSA-K scandium chloride Chemical compound Cl[Sc](Cl)Cl DVMZCYSFPFUKKE-UHFFFAOYSA-K 0.000 claims abstract description 53
- 239000002253 acid Substances 0.000 claims abstract description 46
- 239000000376 reactant Substances 0.000 claims abstract description 45
- 229920002545 silicone oil Polymers 0.000 claims abstract description 44
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 72
- 229910052786 argon Inorganic materials 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims 2
- 229920002379 silicone rubber Polymers 0.000 abstract description 40
- 238000002390 rotary evaporation Methods 0.000 description 39
- 239000004945 silicone rubber Substances 0.000 description 28
- 230000000694 effects Effects 0.000 description 16
- 238000007605 air drying Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 13
- 229910021641 deionized water Inorganic materials 0.000 description 13
- 238000005303 weighing Methods 0.000 description 12
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 230000003197 catalytic effect Effects 0.000 description 7
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 6
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000007711 solidification Methods 0.000 description 5
- 238000004073 vulcanization Methods 0.000 description 5
- NHRXFCLMFQSGIM-UHFFFAOYSA-N P(=O)(O)(O)O.ClC=C.ClC=C.ClC=C Chemical compound P(=O)(O)(O)O.ClC=C.ClC=C.ClC=C NHRXFCLMFQSGIM-UHFFFAOYSA-N 0.000 description 4
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000723347 Cinnamomum Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000017803 cinnamon Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of catalysts, and particularly discloses a single-component platinum catalyst and a preparation method thereof. The preparation method of the single-component platinum catalyst comprises the following steps: step 1), uniformly mixing chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water to obtain a premix; step 2), heating the premix to 76-78 ℃, and stirring and reacting for 10-12 hours to obtain a reactant; and 3) heating, concentrating and drying the reactant to obtain the single-component platinum catalyst. The invention has the advantage of improving the strength of the silicon rubber.
Description
Technical Field
The invention relates to the field of catalysts, in particular to a single-component platinum catalyst and a preparation method thereof.
Background
The platinum catalyst is a catalyst prepared by taking metal platinum as a main active component, and can be used as a catalyst of liquid addition type silicone rubber.
The liquid silicone rubber is liquid before re-solidification, has extremely high plasticity, can form various complicated shapes, can be slowly solidified at normal temperature after adding the catalyst, can be rapidly solidified under the heating condition, has more application scenes, and is applied to a plurality of fields.
Although the liquid silicone rubber has high plasticity, the strength after curing is low when a common platinum catalyst is added, so that the application of the liquid silicone rubber is still greatly limited, and therefore, there is room for improvement.
Disclosure of Invention
In order to improve the strength of the silicone rubber, the application provides a single-component platinum catalyst and a preparation method thereof.
In a first aspect, the present application provides a preparation method of a single-component platinum catalyst, which adopts the following technical scheme:
the preparation method of the single-component platinum catalyst comprises the following steps:
step 1), uniformly mixing chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water to obtain a premix;
step 2), heating the premix to 76-78 ℃, and stirring and reacting for 10-12 hours to obtain a reactant;
and 3) heating, concentrating and drying the reactant to obtain the single-component platinum catalyst.
Through adopting above-mentioned technical scheme, through with chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine, water misce bene, at 76-78 ℃, stirring reaction is 10-12h makes each component mutually react the cooperation, and the platinum catalyst that prepares has better catalytic activity, can make the vulcanization density of silicone rubber higher simultaneously to the tensile strength that makes silicone rubber is showing and is improving, makes the intensity after the liquid silicone rubber solidification higher, can be applicable to the application scenario of high strength demand better.
Preferably, the mass ratio of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine is 59-61:3.9-4.1:2.9-3.1:6.2-6.4:3.5-3.7.
Through adopting above-mentioned technical scheme, through the mass proportion of specifically selecting chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine for each component mutually reaction complex effect is better, improves the crosslinked density when liquid silicone rubber solidification better, makes liquid silicone rubber have higher intensity after solidifying, and the quality is better, is better suitable for high-strength application environment better.
Preferably, the mass ratio of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water is 59-61:3.9-4.1:2.9-3.1:6.2-6.4:3.5-3.7:100.
through adopting above-mentioned technical scheme, through the mass proportion of specifically selecting chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine, water for each component is fully dissolved in water, thereby can fully react the cooperation under the heating condition, the platinum catalyst of preparation can improve the crosslinked density of silicone rubber better, and is better to the modification effect of silicone rubber.
Preferably, in the step 2), argon is continuously introduced during the stirring reaction.
Through adopting above-mentioned technical scheme, through letting in the argon gas, can play better catalytic action for chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine mutually react complex effect is better, and the quality of the platinum catalyst of preparation is higher, and is better to the modification effect of silicone rubber.
Preferably, the argon gas is introduced into the reactor in an amount of 1-2ml of argon gas per minute in 1kg of water.
Through adopting above-mentioned technical scheme, through the introduction amount of concrete selection wool argon gas for catalytic chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine mutually react complex effect is better, reduces the argon gas consumption simultaneously, has higher economic value.
Preferably, in the step 3), spin-evaporation concentration is adopted during heating concentration, and the spin-evaporation temperature is 60-65 ℃.
Through adopting above-mentioned technical scheme, through adopting spin concentration for concentrating the temperature decline for platinum catalyst can be better with the separation of water, the platinum catalyst water content of obtaining is lower, when being applied to in the silicone rubber, can effectively reduce the phenomenon that the silicone rubber produced the bubble, and the cured silicone rubber quality is better.
Preferably, in the step 3), the air is dried naturally at room temperature.
Through adopting above-mentioned technical scheme, through natural air drying, the effect that reduces the water content in the platinum catalyst is better, can reduce the energy effect moreover, has higher economic value, reduces environmental pollution.
In a second aspect, the present application provides a single-component platinum catalyst, which adopts the following technical scheme:
a single-component platinum catalyst is prepared by the preparation method of the single-component platinum catalyst.
Through adopting above-mentioned technical scheme, single component platinum catalyst can realize the slow vulcanization of room temperature and the quick vulcanization of high temperature to addition type liquid silicone rubber, and catalytic activity is higher, and the quantity is less, can effectively improve the crosslink density of silicone rubber simultaneously for the intensity after the silicone rubber solidification is showing and is improving, and then realizes the modification to the silicone rubber intensity, makes the silicone rubber can be better applied to the scene that high strength required, and the application restriction is less, and the range of application is wider.
In summary, the present application has the following beneficial effects:
1. according to the method, chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water are uniformly mixed, and the components are mutually reacted and matched by stirring and reacting for 10-12 hours at the temperature of 76-78 ℃, so that the prepared platinum catalyst has good catalytic activity, and meanwhile, the vulcanization density of the silicone rubber is higher, so that the tensile strength of the silicone rubber is obviously improved, the strength of the cured liquid silicone rubber is higher, and the method can be better suitable for application scenes with high strength requirements.
2. In the application, the mass ratio of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine is preferably selected, so that the mutual reaction and matching effects of the components are better, the crosslinking density of the liquid silicone rubber during curing is better improved, the liquid silicone rubber has higher strength after curing, the quality is better, and the liquid silicone rubber is better suitable for a high-strength application environment.
3. In this application, preferably through the lets in the argon gas, can play better catalytic action for chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine mutually react the complex effect better, the platinum catalyst's that makes quality is higher, and is better to the modification effect of silicone rubber.
Detailed Description
The present application is described in further detail below with reference to examples.
Example 1
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), 59g of chloroplatinic acid, 3.9g of scandium chloride, 2.9g of ruthenium chloride, 6.2g of water-soluble silicone oil, 3.5g of piperazine and 100g of deionized water are weighed, the rotating speed is 120r/min, and stirring is carried out for 10min, and the premix is obtained after uniform mixing.
And 2) heating the premix to 76 ℃, introducing argon, introducing 0.1ml of argon per minute, and continuously stirring for reaction for 10 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 60 ℃, the rotary evaporation pressure is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 2
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 3
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 61g of chloroplatinic acid, 4.1g of scandium chloride, 3.1g of ruthenium chloride, 6.4g of water-soluble silicone oil, 3.7g of piperazine and 100g of deionized water, stirring at a rotating speed of 120r/min for 10min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 78 ℃, introducing argon with the argon introducing amount of 0.2ml of argon per minute, and continuously stirring for reaction for 12 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 65 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 4
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 2g of scandium chloride, 5g of ruthenium chloride, 4g of water-soluble silicone oil, 5.9g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 5
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 6g of scandium chloride, 1g of ruthenium chloride, 8g of water-soluble silicone oil, 1.9g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 6
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 70 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain a reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 7
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.05ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Example 8
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃ at the rotating speed of 120r/min, and continuously stirring and reacting for 11h to obtain a reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Comparative example 1
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of potassium chlorate, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Wherein, potassium chlorate comes from the market, CAS number: 3811-04-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Comparative example 2
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of stannic chloride, 6.3g of water-soluble silicone oil, 3.6g of piperazine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, tin tetrachloride is commercially available and has CAS number: 7646-78-8.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Comparative example 3
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of tris (2-chloroethylene) phosphate, 3.6g of piperazine and 100g of deionized water, stirring at the rotating speed of 120r/min for 10min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Among them, tris (2-chloroethylene) phosphate is commercially available as CAS: 115-96-8.
Wherein, piperazine is from commercial, CAS number: 110-85-0.
Comparative example 4
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of scandium chloride, 3g of ruthenium chloride, 6.3g of water-soluble silicone oil, 3.6g of pyrimidine and 100g of deionized water, stirring for 10min at a rotating speed of 120r/min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Scandium chloride is commercially available, CAS number: 10361-84-9.
Among them, ruthenium chloride is commercially available and has CAS number: 14898-67-0.
Wherein, the water-soluble silicone oil is purchased from Shandong Xin Runjin chemical industry Co., ltd, model JN-204.
Among them, pyrimidine is commercially available from CAS number: 289-95-2.
Comparative example 5
A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), weighing 60g of chloroplatinic acid, 4g of potassium chlorate, 3g of stannic chloride, 6.3g of tris (2-chloroethylene) phosphate, 3.6g of pyrimidine and 100g of deionized water, stirring at the rotating speed of 120r/min for 10min, and uniformly mixing to obtain a premix.
And 2) heating the premix to 77 ℃, introducing argon, introducing 0.15ml of argon per minute, and continuously stirring for reacting for 11 hours at the rotating speed of 120r/min to obtain the reactant.
And 3) concentrating the reactant by rotary evaporation, wherein the rotary evaporation temperature is 63 ℃, the rotary evaporation force is 0.01MPa, concentrating the reactant into paste, and naturally air-drying the paste at room temperature to obtain the single-component platinum catalyst.
Among them, chloroplatinic acid is commercially available and has CAS number: 16941-12-1.
Wherein, potassium chlorate comes from the market, CAS number: 3811-04-9.
Among them, tin tetrachloride is commercially available and has CAS number: 7646-78-8.
Among them, tris (2-chloroethylene) phosphate is commercially available as CAS: 115-96-8.
Among them, pyrimidine is commercially available from CAS number: 289-95-2.
Experiment 1
The tensile strength of the test specimen to which the one-component platinum catalysts of each example and comparative example were added was measured according to GB/T528-2009 "measurement of tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber".
The preparation method of the sample to be tested comprises the following steps:
100g of vinyl silicone oil, 2.5g of hydrogen-containing silicone oil at the end and 1g of single-component platinum catalyst are weighed, uniformly mixed, injected into a mold, heated and pressurized for solidification, at 120 ℃, under 10MPa, for 100s of vulcanization time, and demoulded to obtain a sample to be tested.
The specific test data for experiment 1 are detailed in table 1.
Table 1.
| Tensile Strength (MPa) | |
| Example 1 | 16.8 |
| Example 2 | 17.1 |
| Example 3 | 16.9 |
| Example 4 | 15.7 |
| Example 5 | 15.9 |
| Example 6 | 15.2 |
| Example 7 | 16.5 |
| Example 8 | 16.3 |
| Comparative example 1 | 14.7 |
| Comparative example 2 | 14.4 |
| Comparative example 3 | 14.2 |
| Comparative example 4 | 14.6 |
| Comparative example 5 | 14.1 |
According to the data comparison of each example and the comparative example in table 1, the tensile strength of each example is obviously higher than that of each comparative example, and it can be seen that the platinum catalyst prepared by compounding chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine in each example has good catalytic activity, and meanwhile, the crosslinking density of the silicone rubber can be effectively improved, so that the tensile strength of the silicone rubber is obviously improved, the silicone rubber can be better applied to high-strength use fields, the application range of the silicone rubber is wider, and the economic value is higher.
As can be seen from the comparison of the data in Table 1 for examples 1-3 and examples 4-5, the tensile strength of the silicone rubber of examples 1-3 is higher than that of examples 4-5, and it can be seen that when chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine are compounded in a specific ratio, the platinum catalyst prepared can better increase the crosslinking density of the cinnamon street, resulting in a higher tensile strength of the silicone rubber.
As can be seen from a comparison of the data of examples 1-3 and example 6 in Table 1, the tensile strength of the silicone rubber of examples 1-3 is higher than that of example 6, and it is seen that the effect of the reaction of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine with each other is reduced when the reaction temperature is lower than 76 ℃, resulting in a reduction in the effect of improving the crosslinking density of the silicone rubber, and thus in a reduction in the effect of modifying the tensile strength of the silicone rubber.
As can be seen from the comparison of the data of examples 1-3 and examples 7-8 in Table 1, the tensile strength of the silicone rubber of examples 1-3 is higher than that of examples 7-8, and it can be seen that the effect of the reaction of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine can be improved by introducing argon, and the effect of the reaction of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine can be better improved by introducing specific argon, so that the effect of the prepared platinum catalyst for improving the tensile strength of the silicone rubber is better.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (8)
1. A preparation method of a single-component platinum catalyst is characterized by comprising the following steps: the method comprises the following steps:
step 1), uniformly mixing chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water to obtain a premix;
step 2), heating the premix to 76-78 ℃, and stirring and reacting for 10-12 hours to obtain a reactant;
and 3) heating, concentrating and drying the reactant to obtain the single-component platinum catalyst.
2. The method for preparing a single-component platinum catalyst according to claim 1, wherein the method comprises the following steps: the mass ratio of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil and piperazine is 59-61:3.9-4.1:2.9-3.1:6.2-6.4:3.5-3.7.
3. The method for preparing a single-component platinum catalyst according to claim 2, wherein the method comprises the following steps: the mass ratio of chloroplatinic acid, scandium chloride, ruthenium chloride, water-soluble silicone oil, piperazine and water is 59-61:3.9-4.1:2.9-3.1:6.2-6.4:3.5-3.7:100.
4. the method for preparing a single-component platinum catalyst according to claim 1, wherein the method comprises the following steps: in the step 2), argon is continuously introduced in the stirring reaction process.
5. The method for preparing a single-component platinum catalyst according to claim 4, wherein the method comprises the following steps: the argon gas is introduced into the water in an amount of 1-2ml per minute per 1kg of water.
6. The method for preparing a single-component platinum catalyst according to claim 1, wherein the method comprises the following steps: in the step 3), spin evaporation concentration is adopted during heating concentration, and the spin evaporation temperature is 60-65 ℃.
7. The method for preparing a single-component platinum catalyst according to claim 6, wherein the method comprises the following steps: in the step 3), the air is dried naturally at room temperature during drying.
8. A single-component platinum catalyst is characterized in that: prepared by the method for preparing the single-component platinum catalyst as claimed in any one of claims 1 to 7.
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