1. A method for preparing a platinum complex, comprising the steps of:

s1, weighing 0.5-1.5 parts of chloroplatinic acid and 57-65 parts of tetramethyl divinyl disiloxane in parts by weight, and mixing to obtain a mixture A;

s2, heating the mixture A to 115-120 ℃, and then ventilating and stirring for 1-2h to prepare a crude platinum complex;

s3, filtering the crude platinum complex prepared in the S2 into a separating funnel, washing with water for injection, and separating black precipitates to obtain light yellow liquid;

s4, after the light yellow liquid in S3 is washed to the PH value of 7.0, the platinum complex is prepared.

2. The method for preparing the platinum complex as claimed in claim 1, wherein the step of pretreating chloroplatinic acid in S1 comprises the following steps:

weighing 0.5-1.5 parts of chloroplatinic acid by weight, and mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: (5-10): (0.5-0.8), and heating to 30-40 ℃ to prepare the acetone solution of chloroplatinic acid.

3. The method for preparing the platinum complex as claimed in claim 2, wherein the step of pretreating the tetramethyldivinyldisiloxane is further included in the step of S1, and the method comprises the following steps:

57-65 parts of tetramethyl divinyl disiloxane is weighed according to the parts by weight, and then the volume ratio is 1: (0.03-0.05) introducing nitrogen and acetylene at the flow rate of 0.25-0.75L/min, heating to 40-50 deg.C, and preheating for 5-10 min.

4. The method for preparing the platinum complex as claimed in claim 3, wherein the specific preparation steps of S1 are as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 0.5-1h in a constant current titration mode at the rotating speed of 150-180r/min, and heating to 50-60 ℃ to obtain a mixture A.

5. The method for preparing the platinum complex as claimed in claim 1, wherein the specific preparation steps of S2 are as follows:

heating the mixture A to 115-120 ℃, and stirring and reacting at the rotating speed of 210-240r/min for 1-2h, wherein the volume ratio in the reaction process is 1: (0.1-0.2) introducing nitrogen and acetylene at a flow rate of 0.25-0.75L/min to obtain crude platinum complex.

6. The method for preparing the platinum complex as claimed in claim 1, wherein the specific preparation steps of S3 are as follows:

filtering the crude platinum complex prepared in S2 into a separating funnel, washing with water for injection at 70-80 ℃, pouring the water for injection according to 86-90% of the volume ratio of the separating funnel, and separating black precipitate.

7. The method of claim 6, wherein the step S3 is repeated 10-16 times to separate the black precipitate from the light yellow liquid from the separating funnel.

8. The method for preparing the platinum complex as claimed in claim 6, wherein the specific preparation steps of S4 are as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 10-12h in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

9. Use of a platinum complex as claimed in any one of claims 1 to 8, characterized in that the platinum complex is used as a catalyst in the synthesis of silicone rubbers.

Background

The platinum complex, i.e. the product obtained by the complexation reaction of platinum Pt [ O-VI ] and ligands such as Cl, NH3, CN, NO2, PR3, CO and the like, wherein the vinyl platinum catalyst is taken as an example, the catalyst mainly takes zero-valent platinum as a main active component, and the catalyst is colorless transparent or light yellow liquid. The catalyst has high catalytic efficiency, can catalyze hydrosilylation vulcanization reaction of vinyl siloxane and hydrogen-containing siloxane at low temperature or high temperature, and has the advantages of no side reaction product, high vulcanization degree and small shrinkage rate in the vulcanization process. Therefore, the method is widely applied to various hydrosilylation reactions, and a high-purity and high-transparency silicone rubber product is easily prepared.

The catalyst specially used for hydrosilylation, that is, the platinum complex, in the related art includes chloroplatinic acid and divinyltetramethyldisiloxane, but the catalyst is a catalyst which is obtained by simply mixing the two, and a vinyl platinum complex cannot be well formed, and the yield is low.

Disclosure of Invention

In order to improve the yield and quality of the platinum complex, the application provides a preparation method and application of the platinum complex.

The preparation method and the application of the platinum complex provided by the application adopt the following technical scheme:

in a first aspect, the present application provides a method for preparing a platinum complex, which adopts the following technical scheme:

a method for preparing a platinum complex, comprising the steps of:

s1, weighing 0.5-1.5 parts of chloroplatinic acid and 57-65 parts of tetramethyl divinyl disiloxane in parts by weight, and mixing to obtain a mixture A;

s2, heating the mixture A to 115-120 ℃, and then ventilating and stirring for 1-2h to prepare a crude platinum complex;

s3, filtering the crude platinum complex prepared in the S2 into a separating funnel, washing with water for injection, and separating black precipitates to obtain light yellow liquid;

s4, after the light yellow liquid in S3 is washed to the PH value of 7.0, the platinum complex is prepared.

By adopting the technical scheme, the chloroplatinic acid and the tetramethyl divinyl disiloxane which are proportioned have the advantages of highest addition reaction degree, better complexing effect, moderate decomposition rate and capability of fully complexing the tetramethyl divinyl disiloxane and the simple substance platinum, and the temperature condition and the reaction duration are favorable for fully decomposing the simple substance platinum by the chloroplatinic acid, so that the yield of the product is ensured.

Preferably, the step S1 further includes a step of pretreatment of chloroplatinic acid, which includes the following steps:

weighing 0.5-1.5 parts of chloroplatinic acid by weight, and mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: (5-10): (0.5-0.8), and heating to 30-40 ℃ to prepare the acetone solution of chloroplatinic acid.

By adopting the technical scheme, the chloroplatinic acid heated and mixed with acetone and divinyl glycol has better dispersibility, higher conversion rate and easier, stable and durable decomposition of simple substance platinum, is favorable for full absorption and complexation of tetramethyl divinyl disiloxane on the simple substance platinum, and ensures the yield of products.

Preferably, the S1 further comprises a pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows: 57-65 parts of tetramethyl divinyl disiloxane is weighed according to the parts by weight, and then the volume ratio is 1: (0.03-0.05) introducing nitrogen and acetylene at the flow rate of 0.25-0.75L/min, heating to 40-50 deg.C, and preheating for 5-10 min.

By adopting the technical scheme, after the nitrogen and the acetylene are introduced, the tetramethyldivinyl disiloxane is matched with preheating treatment, so that the absorption and complexation performance is stronger, the decomposed simple substance platinum can be fully and effectively combined, the generation of platinum black is reduced to a certain extent by introducing a small amount of acetylene gas, and the reduction of the yield of the product caused by too slow complexation or incomplete reaction is not easy to occur.

Preferably, the specific preparation steps of S1 are as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 0.5-1h in a constant current titration mode at the rotating speed of 150-180r/min, and heating to 50-60 ℃ to obtain a mixture A.

By adopting the technical scheme and adopting a constant-current titration mode, the reaction rate can be controlled within a relatively reasonable range all the time, the phenomenon that elemental platinum is not absorbed and complexed timely due to too low reaction speed or insufficient combination is caused due to too fast reaction is reduced, platinum black is not easy to generate, and the product yield is ensured.

Preferably, the specific preparation steps of S2 are as follows:

heating the mixture A to 115-120 ℃, and stirring and reacting at the rotating speed of 210-240r/min for 1-2h, wherein the volume ratio in the reaction process is 1: (0.1-0.2) introducing nitrogen and acetylene at a flow rate of 0.25-0.75L/min to obtain crude platinum complex.

By adopting the technical scheme, when the reaction is carried out under the conditions of the rotating speed and the temperature, the complexing effect of the chloroplatinic acid and the tetramethyl divinyl disiloxane in the mixture A is the best, and a small amount of acetylene is introduced, so that a platinum simple substance can be better absorbed and complexed by the tetramethyl divinyl disiloxane, the platinum black is not easy to generate, the forward reaction is facilitated, and the product yield is further ensured.

Preferably, the specific preparation steps of S3 are as follows:

filtering the crude platinum complex prepared in S2 into a separating funnel, washing with water for injection at 70-80 ℃, pouring the water for injection according to 86-90% of the volume ratio of the separating funnel, and separating black precipitate.

By adopting the technical scheme, the purity of the crude platinum complex separated by the steps is higher, so that the catalytic efficiency is not easily influenced by invalid components or impurities in the catalyst during the subsequent catalysis, and the catalytic activity and the purity of the catalyst are ensured.

Preferably, the above step S3 is repeated 10-16 times to separate the black precipitate from the light yellow liquid from the separatory funnel.

By adopting the technical scheme, the crude platinum complex repeatedly separated by the steps has high purity, and ineffective components or impurities in the crude platinum complex can be sufficiently removed, so that the catalytic efficiency and catalytic activity of the platinum complex are ensured.

Preferably, the specific preparation steps of S4 are as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 10-12h in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

By adopting the technical scheme, black precipitates and impurities in the faint yellow liquid after vacuum standing can be further separated out, so that the purity and the catalytic efficiency of the platinum complex are further ensured, and the phenomenon of catalytic toxicity caused by the impurities or ineffective substances is not easy to occur.

In a second aspect, the present application provides an application of a platinum complex, which adopts the following technical scheme:

the use of a platinum complex as a catalyst in the synthesis of silicone rubber.

By adopting the technical scheme, the prepared platinum complex can be used for hydrosilylation reaction, namely, silicon rubber synthesis, the synthesis efficiency is higher, and the performance of the synthesized product is more stable.

In summary, the present application has the following beneficial effects:

1. according to the preparation method, the chloroplatinic acid and the tetramethyldivinyldisiloxane in the ratio are matched with the temperature condition and the reaction duration, so that the chloroplatinic acid can be fully decomposed into simple substance platinum, the decomposition rate is moderate, the simple substance platinum can be fully absorbed and complexed by the tetramethyldivinyldisiloxane, and the yield of the product is ensured;

2. according to the method, chloroplatinic acid, acetone and divinyl glycol are heated and mixed, so that the chloroplatinic acid is better in dispersibility and higher in conversion rate, simple substance platinum complexed with tetramethyl divinyl disiloxane can be stably and durably decomposed, and the yield of the product is further guaranteed;

3. according to the method, nitrogen and acetylene are introduced into the tetramethyldivinyldisiloxane, and are matched with preheating treatment, so that the absorption and complexation performance of the tetramethyldivinyldisiloxane is greatly improved, the decomposed simple substance platinum can be fully and effectively combined, the platinum black is not easy to generate, and the yield of the product is ensured;

4. this application is through in mixture A heating stirring process, and conditions such as control temperature, rotational speed and acetylene input have ensured the complexation effect of this step, and platinum simple substance can be better by the absorption complexation of tetramethyl divinyl disiloxane, is difficult for producing platinum black, then the yield of product can maintain at higher level.

Detailed Description

The present application will be described in further detail with reference to examples.

Examples of the present applicationThe starting materials and equipment used in the examples were all commercially available except as specified below: chloroplatinic acid, purchased from chemical reagents of national pharmaceutical group, Inc., having the formula H₁₄Cl₆O₆The molecular weight of Pt is 517.9096, and the platinum content of chloroplatinic acid is not less than 37.0%;

tetramethyldiethylenedisiloxane, available from Zhejiang Quzhou Jian orange Silicone Co., Ltd, of formula C₈H₁₈OSi₂The vinyl content of the tetramethyldivinyldisiloxane is not less than 27 percent, and the refractive index (n) of the tetramethyldivinyldisiloxane is_D ²⁰) 1.400 to 1.413, specific gravity of tetramethyldivinyldisiloxane (d)₄ ²⁰) Is 0.800-0.830g/cm³；

Ventilator, model LBN49-3, purchased from bebo purification technologies, inc, changzhou;

cooling water installation model XIIT-50D, purchased from Shanghai billow refrigeration appliances, Inc.

Examples

Example 1

S1, weighing 5g of chloroplatinic acid, adding the chloroplatinic acid into a 1000ml three-neck flask, weighing 570g of tetramethyl divinyl disiloxane, adding the tetramethyldivinyl disiloxane into the 1000ml three-neck flask, mixing the tetramethyldivinyl disiloxane and the chloroplatinic acid for 0.25h at the rotating speed of 130r/min, and heating to 40 ℃ to obtain a mixture A;

s2, transferring the three-neck flask containing the mixture A in the S1 into an oil bath, heating to 115 ℃, and stirring at the rotating speed of 200r/min for reaction for 1h, wherein the volume ratio of the mixture A to the mixture B in the reaction process is 1: introducing nitrogen and acetylene at the flow rate of 0.1L/min to 0.05 to obtain light yellow liquid, i.e. crude platinum complex;

s3, filtering the crude platinum complex prepared in the S2 into a 1000ml separating funnel, washing with water for injection at 60 ℃, pouring the water for injection into the separating funnel according to 84% of the volume ratio of the separating funnel, separating black precipitates, repeating the step S3 for 8 times, and separating to obtain light yellow liquid;

s4, after the light yellow liquid in the S4 is washed until the pH value is 7.0 by using a precise pH test paper, standing for 8 hours, and filtering out black precipitates by using filter paper to prepare the platinum complex.

Examples 2 to 6

A method for preparing a platinum complex, which is different from example 1 in that each component and the corresponding weight thereof are shown in table 1.

TABLE 1 Components and weights (g) thereof in examples 1-6

Example 7

The preparation method of the platinum complex is different from the preparation method of the embodiment 3 in that S1 further comprises the pretreatment of chloroplatinic acid, and the specific steps are as follows:

after weighing chloroplatinic acid according to the corresponding weight, mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: 2.5: 0.3, and heating to 20 ℃ to obtain an acetone solution of chloroplatinic acid.

Example 8

The preparation method of the platinum complex is different from the preparation method of the embodiment 3 in that S1 further comprises the pretreatment of chloroplatinic acid, and the specific steps are as follows:

after weighing chloroplatinic acid according to the corresponding weight, mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: 5: 0.5, and heated to 30 ℃ to obtain an acetone solution of chloroplatinic acid.

Example 9

The preparation method of the platinum complex is different from the preparation method of the embodiment 3 in that S1 further comprises the pretreatment of chloroplatinic acid, and the specific steps are as follows:

after weighing chloroplatinic acid according to the corresponding weight, mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: 7.5: 0.65, and heated to 35 ℃ to obtain an acetone solution of chloroplatinic acid.

Example 10

The preparation method of the platinum complex is different from the preparation method of the embodiment 3 in that S1 further comprises the pretreatment of chloroplatinic acid, and the specific steps are as follows:

after weighing chloroplatinic acid according to the corresponding weight, mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: 10: 0.8, and heated to 40 ℃ to obtain an acetone solution of chloroplatinic acid.

Example 11

The preparation method of the platinum complex is different from the preparation method of the embodiment 3 in that S1 further comprises the pretreatment of chloroplatinic acid, and the specific steps are as follows:

after weighing chloroplatinic acid according to the corresponding weight, mixing the chloroplatinic acid with acetone and divinyl glycol according to the weight ratio of 1: 12.5: 1, mixing and heating to 50 ℃ to prepare an acetone solution of chloroplatinic acid.

Example 12

The difference between the preparation method of the platinum complex and the preparation method of the platinum complex in example 9 is that S1 further comprises the pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows:

weighing tetramethyldivinyldisiloxane according to the corresponding weight, and then mixing the components in a volume ratio of 1: introducing nitrogen and acetylene at the flow rate of 0.01L/min, heating to 30 deg.C, and preheating for 2.5 min.

Example 13

The difference between the preparation method of the platinum complex and the preparation method of the platinum complex in example 9 is that S1 further comprises the pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows:

weighing tetramethyldivinyldisiloxane according to the corresponding weight, and then mixing the components in a volume ratio of 1: 0.03 introducing nitrogen and acetylene at the flow rate of 0.25L/min, heating to 40 deg.C, and preheating for 5 min.

Example 14

The difference between the preparation method of the platinum complex and the preparation method of the platinum complex in example 9 is that S1 further comprises the pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows:

weighing tetramethyldivinyldisiloxane according to the corresponding weight, and then mixing the components in a volume ratio of 1: 0.04 and 0.50L/min of nitrogen and acetylene, and preheating for 7.5min at 45 ℃.

Example 15

The difference between the preparation method of the platinum complex and the preparation method of the platinum complex in example 9 is that S1 further comprises the pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows:

weighing tetramethyldivinyldisiloxane according to the corresponding weight, and then mixing the components in a volume ratio of 1: 0.05 introducing nitrogen and acetylene at the flow rate of 0.75L/min, heating to 50 deg.C, and preheating for 10 min.

Example 16

The difference between the preparation method of the platinum complex and the preparation method of the platinum complex in example 9 is that S1 further comprises the pretreatment of tetramethyldivinyldisiloxane, and the specific steps are as follows:

weighing tetramethyldivinyldisiloxane according to the corresponding weight, and then mixing the components in a volume ratio of 1: 0.1 introducing nitrogen and acetylene with the flow rate of 1.0L/min, heating to 60 deg.C, and preheating for 12.5 min.

Example 17

A method for preparing a platinum complex, which is different from example 14 in that S1 is specifically prepared as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 0.25h in a constant current titration mode at the rotating speed of 130r/min, and heating to 40 ℃ to obtain a mixture A.

Example 18

A method for preparing a platinum complex, which is different from example 14 in that S1 is specifically prepared as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 0.5h in a constant current titration mode at the rotating speed of 150r/min, and heating to 50 ℃ to obtain a mixture A.

Example 19

A method for preparing a platinum complex, which is different from example 14 in that S1 is specifically prepared as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 0.75h in a constant current titration mode at the rotating speed of 165r/min, and heating to 55 ℃ to obtain a mixture A.

Example 20

A method for preparing a platinum complex, which is different from example 14 in that S1 is specifically prepared as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 1 hour at the rotating speed of 180r/min by adopting a constant current titration mode, and heating to 60 ℃ to prepare a mixture A.

Example 21

A method for preparing a platinum complex, which is different from example 14 in that S1 is specifically prepared as follows:

mixing the acetone solution of chloroplatinic acid and the pretreated tetramethyl divinyl disiloxane for 1.25h in a constant current titration mode at the rotating speed of 200r/min, and heating to 70 ℃ to obtain a mixture A.

Example 22

A method for preparing a platinum complex, which is different from example 14 in that S2 is specifically prepared as follows:

transferring the three-neck flask containing the mixture A in S1 into an oil bath, heating to 115 ℃, and stirring at the rotating speed of 210r/min for reaction for 1h, wherein the volume ratio of the mixture A to the mixture B in the reaction process is 1: 0.1 introduction of nitrogen and acetylene at a flow rate of 0.25L/min to obtain a pale yellow liquid, i.e., a crude platinum complex.

Example 23

A method for preparing a platinum complex, which is different from example 14 in that S2 is specifically prepared as follows:

transferring the three-neck flask containing the mixture A in S1 into an oil bath, heating to 117.5 ℃, and stirring at 225r/min for reaction for 1.5h, wherein the volume ratio of the mixture A to the mixture B in the reaction process is 1: 0.15 introduction of nitrogen and acetylene at a flow rate of 0.50L/min to obtain a pale yellow liquid, i.e., a crude platinum complex.

Example 24

A method for preparing a platinum complex, which is different from example 14 in that S2 is specifically prepared as follows:

transferring the three-neck flask containing the mixture A in S1 into an oil bath, heating to 120 ℃, and stirring at the rotating speed of 240r/min for reaction for 2 hours, wherein the volume ratio of the mixture A to the mixture B in the reaction process is 1: 0.2 introduction of nitrogen and acetylene at a flow rate of 0.75L/min to obtain a pale yellow liquid, i.e., a crude platinum complex.

Example 25

A method for preparing a platinum complex, which is different from example 14 in that S2 is specifically prepared as follows:

transferring the three-neck flask containing the mixture A in S1 into an oil bath, heating to 120 ℃, and stirring at the rotating speed of 250r/min for reaction for 2 hours, wherein the volume ratio of the mixture A to the mixture B in the reaction process is 1: 0.25 of the reaction solution was purged with nitrogen and acetylene at a flow rate of 1.0L/min to obtain a pale yellow liquid, i.e., a crude platinum complex.

Example 26

A method for preparing a platinum complex, which is different from example 1 in that S3 is specifically prepared as follows:

and (3) filtering the crude platinum complex prepared in the S2 into a 1000ml separating funnel, washing with water for injection at 70 ℃, pouring the water for injection into the separating funnel according to 86% of the volume ratio of the separating funnel, separating black precipitate, and separating to obtain light yellow liquid.

Example 27

A method for preparing a platinum complex, which is different from example 1 in that S3 is specifically prepared as follows:

and (3) filtering the crude platinum complex prepared in the S2 into a 1000ml separating funnel, washing with water for injection at 75 ℃, pouring the water for injection into the separating funnel according to 88% of the volume ratio of the separating funnel, separating black precipitate, and separating to obtain light yellow liquid.

Example 28

A method for preparing a platinum complex, which is different from example 1 in that S3 is specifically prepared as follows:

and (3) filtering the crude platinum complex prepared in the S2 into a 1000ml separating funnel, washing with water for injection at 80 ℃, pouring the water for injection into the separating funnel according to 90% of the volume ratio of the separating funnel, separating black precipitate, and separating to obtain light yellow liquid.

Example 29

A method for preparing a platinum complex, which is different from example 1 in that S3 is specifically prepared as follows:

and (3) filtering the crude platinum complex prepared in the S2 into a 1000ml separating funnel, washing with water for injection at 90 ℃, pouring the water for injection into the separating funnel according to 92% of the volume ratio of the separating funnel, separating black precipitate, and separating to obtain light yellow liquid.

Example 30

A method for preparing a platinum complex, which is different from example 1 in that the above-described S3 procedure was repeated 10 times, and a black precipitate in a pale yellow liquid was separated from a separatory funnel.

Example 31

A method for preparing a platinum complex, which is different from example 1 in that the above-described S3 procedure was repeated 13 times, and a black precipitate in a pale yellow liquid was separated from a separatory funnel.

Example 32

A method for preparing a platinum complex, which is different from example 1 in that the above-described S3 procedure was repeated 16 times, and a black precipitate in a pale yellow liquid was separated from a separatory funnel.

Example 33

A method for preparing a platinum complex, which is different from example 1 in that the above-described S3 procedure was repeated 18 times, and a black precipitate in a pale yellow liquid was separated from a separatory funnel.

Example 34

A method for preparing a platinum complex, which is different from example 1 in that S4 is specifically prepared as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 8 hours in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

Example 35

A method for preparing a platinum complex, which is different from example 1 in that S4 is specifically prepared as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 10 hours in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

Example 36

A method for preparing a platinum complex, which is different from example 1 in that S4 is specifically prepared as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 11 hours in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

Example 37

A method for preparing a platinum complex, which is different from example 1 in that S4 is specifically prepared as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 12 hours in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

Example 38

A method for preparing a platinum complex, which is different from example 1 in that S4 is specifically prepared as follows:

and (3) after the light yellow liquid in the S3 is washed until the pH value is 7.0, standing for 14 hours in a vacuum state, filtering out black precipitates again to obtain the platinum complex.

Comparative example

Comparative example 1

A method for preparing a platinum complex, which is different from example 1 in that the platinum complex is prepared by mixing tetramethyldivinyldisiloxane chloroplatinate at a rotation speed of 130r/min for 0.25 h.

Comparative example 2

A method for preparing a platinum complex, which is different from the method of example 1, is that after the mixture A in S2 is heated to 80 ℃, the mixture A is stirred for 0.5h at the rotating speed of 200r/min, and a crude platinum complex is prepared.

Comparative example 3

A method for preparing a platinum complex, which is different from the method of example 1, is that after the mixture A in S2 is heated to 150 ℃, the mixture A is stirred for 3 hours at the rotating speed of 200r/min, and a crude platinum complex is prepared.

Performance test

Detection method/test method

The platinum complexes obtained in examples 1 to 38 and comparative example 3 were respectively used as test objects, the weights of the obtained products were recorded and examined, and the refractive indices (n) of the obtained platinum complexes were measured_D ²⁰) 1.405-1.415, specific gravity (d)₄ ²⁰) 0.805 to 0.820g/cm³. Yields were obtained based on weight of product/starting material 100% and are reported in table 2 for each group.

230g of octamethylcyclotetrasiloxane, 1g of tetramethyldivinyldisiloxane and 0.1g of platinum complex were weighed out by weight, and a hydrosilylation reaction was carried out at 70 ℃ and the reaction times of the respective groups were recorded after the reaction was completed.

In which the catalytic reaction time in comparative example 1 was taken as a catalytic value of 1 unit, and the catalytic values of each of the groups of examples 1 to 38 were catalytic reaction times of each group/catalytic reaction time in comparative example 1, and the catalytic values of each group are shown in Table 2.

Table 2 results of performance testing

Combining examples 1-6 and table 2, it can be seen that the yields of the platinum complexes prepared in examples 1-6 are all higher than 81%, and the catalytic values are all ≦ 0.89, and it can be seen that the yields of the platinum complexes prepared under the above-mentioned mixing conditions are higher, and the catalytic performance is stronger.

Example 3 is the best example, the weight of the product is 511.4g, the yield is 83.7%, and the catalytic value is only 0.86, thus the mixture ratio is the best mixture ratio.

In conclusion, the components in the proportion are beneficial to full complexation of chloroplatinic acid and tetramethyl divinyl disiloxane, and further the yield and the quality of the product are guaranteed.

Combining example 3, examples 7-11 and table 2, it can be seen that the yields of the platinum complexes prepared in examples 7-11 are all higher than 83.5%, and the catalytic values are all ≦ 0.85, which indicates that the pretreated chloroplatinic acid has a higher conversion rate, and can stably and persistently decompose elemental platinum, thereby ensuring the yield of the product.

Example 9 is the best example with a product weight of 516.3g, a yield of 84.5% and a catalytic value of only 0.84, and the pretreatment process conditions are seen to be the best conditions.

In conclusion, the pretreated chloroplatinic acid has better dispersibility and higher conversion rate, and then the tetramethyldivinyldisiloxane can stably and fully absorb and complex the simple substance platinum, thereby ensuring the yield of the product.

By combining example 9, examples 12 to 16 and table 2, it can be seen that the yields of the platinum complexes prepared in examples 12 to 16 are all higher than 84.5% and the catalytic values are all less than or equal to 0.83, and it can be seen that the pretreated tetramethyldivinyldisiloxane has strong absorption and complexation properties, and can fully complex and decompose simple substance platinum, thereby ensuring the yield of the product.

Example 14 is the best example with a product weight of 523.0g, a yield of 85.6% and a catalytic value of only 0.81, and the pretreatment process conditions are seen to be the best conditions.

In summary, the pretreated tetramethyldivinyldisiloxane has stronger absorption and complexation performance, and is matched with the introduction of a small amount of acetylene, so that the generation of platinum black can be reduced to a certain extent, and incomplete reaction caused by too slow or too fast complexation rate is not easy to occur.

Combining example 14, examples 17-21, comparative example 1 and table 2, it can be seen that the yields of the platinum complexes prepared in examples 17-21 are all higher than 86.0%, and the catalytic values are all less than or equal to 0.80, which indicates that the reaction rate under the process conditions is relatively suitable, and the platinum simple substance can be sufficiently absorbed by tetramethyldivinyldisiloxane.

Example 19 is the best example with a product weight of 538.3g, a yield of 88.1% and a catalytic value of only 0.76, and the process conditions are seen to be the best conditions.

In comparative example 1, since heating and the like were not performed, the weight of the product was only 259.9g, the yield was 45.2%, and the catalytic performance was relatively weak.

In conclusion, the constant-current titration mode is adopted, so that the full reaction is facilitated, simple substance platinum is easy to complex with tetramethyl divinyl disiloxane, and simultaneously, platinum black is not easy to generate, and the yield of the product is further ensured.

By combining example 1, examples 22-25, comparative examples 2-3 and table 2, it can be seen that the yields of the platinum complexes prepared in examples 22-25 are all higher than 86.0% and the catalytic values are all less than or equal to 0.77, which indicates that the platinum simple substance under the process conditions can be fully complexed with the tetramethyldivinyldisiloxane, and platinum black is not easily generated, which is beneficial to improving the yield of the product.

Example 23 is the most preferred example, with a product weight of 532.2g, a yield of 87.1% and a catalytic value of only 0.73, and the process conditions are seen to be the most preferred conditions.

As can be seen from comparative examples 2-3, when the temperature during the reaction is too high or too low, the reaction is not favorable, the product yield is less than 78.5%, and the catalytic performance is relatively weak.

In conclusion, when the reaction is carried out under the conditions of the rotating speed and the temperature, the complexing effect of the chloroplatinic acid and the tetramethyldivinyldisiloxane is the best, and a small amount of acetylene is introduced, so that the platinum simple substance can be better absorbed and complexed by the tetramethyldivinyldisiloxane, the generation of platinum black is reduced, and the yield of the product is further ensured.

Combining example 1, examples 26-38 and Table 2, it can be seen that the yields of the platinum complexes prepared in examples 26-38 are all higher than 80.0% and the catalytic values are all ≦ 0.88. Therefore, the components of the platinum complex subjected to impurity removal by the separation steps are more stable and single, the black precipitate can be fully separated out, the catalytic efficiency is not easily influenced by invalid components or impurities in the catalyst, and the catalytic activity and the purity of the catalyst are guaranteed.

The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.