Preparation method of dibutyl-tin di-neodecanoate

By optimizing the preparation method of dibutyl-dineodecanoate, controlling the purity of raw materials and reaction conditions, the production complexity and environmental pollution problems were solved, and efficient and stable product preparation was achieved. It was suitable for cross-linking reactions of PVC thermal stabilizers and polyurethane.

CN120289513APending Publication Date: 2025-07-11YUNNAN TIN CHEM PROD CO LTD
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Patent Information

Application Number
CN202510445120.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-10
Publication Date
2025-07-11

AI Technical Summary

Technical Problem

The existing dibutyl-dineodecanoate production process is complex, the reaction conditions control requirements are high, the raw materials are hazardous chemicals, resulting in high production costs, unstable product quality, and serious environmental pollution.

Method used

Using strict control of raw material purity and reaction conditions, dibutyl tin oxide is generated through appropriate alkaline liquid catalytic reaction, and then reacted with neodecanoic acid, combined with washing, centrifugation, drying and filtration steps, the reaction process is optimized to obtain high-purity dibutyl-dineodecanoic acid tin.

Benefits of technology

It improves product quality and yield, reduces production costs, ensures the stability and safety of reactions, reduces environmental pollution, and is suitable for industrial production.

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Abstract

The invention discloses a preparation method of dibutyl-tin di-neodecanoate, which specifically comprises the following steps: (1) reacting dibutyltin dichloride with alkali liquor to generate dibutyltin oxide, and then reacting the dibutyltin oxide with neodecanoic acid to obtain a crude product; or, dibutyltin dichloride and neodecanoic acid are mixed firstly, then alkali liquor is dropwise added for a reaction, and a crude product is obtained; and (2) sequentially washing, centrifugally dewatering, drying and filtering the crude product to obtain the product. The preparation method has remarkable advantages, the product quality is stable, the tin content ranges from 20.1% to 20.5%, the chlorine content is lower than 0.1%, the moisture content is lower than 0.7%, and the density and the refractive index conform to expectations; the yield is up to 96% or above, which is far better than that of a traditional process; the process stability is high, and it can be guaranteed that the quality of products of different batches is consistent through amplification and repeated experiment verification; the method is safe and environment-friendly, strictly controls the use of dangerous chemicals, and properly treats three wastes; the cost is reduced, and raw material waste, side reaction and energy and material consumption are reduced.
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Description

Technical Field

[0001] The present invention relates to the technical field of organotin compounds, and more specifically to a preparation method of dibutyl-dineodecanoate tin. Background Art

[0002] Dibutyl-dineodecanoate tin plays an irreplaceable role in many important fields. In the PVC processing industry, dibutyl-dineodecanoate tin is a key heat stabilizer, which can significantly improve the thermal stability, weather resistance, heat resistance and transparency of PVC products, extend the service life of the products, and is widely used in the production of outdoor PVC products. At the same time, in the cross-linking reaction of polyurethane and the condensation reaction of silanol, dibutyl-dineodecanoate tin acts as an efficient catalyst and plays an important role in the manufacture of products such as PU resin slurry, rigid foam, flexible foam, coatings, adhesives and elastomers.

[0003] However, the production of dibutyl-dineodecanoate tin in China currently faces many problems. On the one hand, the organotin production process is complex, involving multiple disciplines, and has extremely high requirements for the control of reaction conditions; on the other hand, some raw materials are dangerous chemicals.

[0004] Therefore, how to develop a preparation method of dibutyl-dineodecanoate tin that is efficient, stable, environmentally friendly and cost controllable is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0005] In view of this, the purpose of the present invention is to provide a preparation method of dibutyl-dineodecanoate tin to solve the deficiencies in the prior art.

[0006] To achieve the above purpose, the present invention adopts the following technical solutions:

[0007] A preparation method of dibutyl-dineodecanoate tin specifically includes the following steps:

[0008] (1) First, react dibutyltin dichloride with an alkali solution to generate dibutyltin oxide, and then react dibutyltin oxide with neodecanoic acid to obtain a crude product;

[0009] Or, first mix dibutyltin dichloride with neodecanoic acid, and then dropwise add an alkali solution to react to obtain a crude product;

[0010] (2) Wash the crude product successively, centrifuge and dehydrate, dry, and filter to obtain the dibutyl-dineodecanoate tin product.

[0011] Specifically, Synthesis Route 1: First, react dibutyltin dichloride with an alkali solution to form dibutyltin oxide. During the reaction, slowly add dibutyltin dichloride to the alkali solution while stirring to ensure full reaction. After the reaction, filter, wash, and dehydrate to obtain pure dibutyltin oxide. Then, mix and react dibutyltin oxide with neodecanoic acid in a reaction kettle. During the reaction process, control the stirring speed and reaction temperature to ensure uniform reaction and obtain a crude product of dibutyl-di-neodecanoate tin.

[0012] Synthesis Route 2: First, uniformly mix dibutyltin dichloride and neodecanoic acid in a mixing kettle, and then slowly add an alkali solution dropwise for reaction. During the dropping process, strictly control the dropping speed and reaction temperature to avoid overly violent reactions. After the reaction, obtain a crude product of dibutyl-di-neodecanoate tin.

[0013] Furthermore, in the above step (1), the purity of dibutyltin dichloride is not less than 99%.

[0014] Furthermore, in the above step (1), the purity of neodecanoic acid is not less than 98%, the impurity content is less than 1%, and the acidity value is 320 - 330.

[0015] The beneficial effect of the above is that high-purity raw materials can reduce the interference of impurities on the reaction, improve reaction selectivity and product quality. At the same time, appropriate acidity helps maintain the stability of the reaction system and promotes the smooth progress of the reaction.

[0016] Furthermore, in the above step (1), the alkali solution is sodium hydroxide solution or potassium hydroxide solution, and the concentration is 2 mol / L.

[0017] The beneficial effect of the above is that the alkali solution plays a catalytic role in the reaction, and appropriate concentration and excess ratio can ensure the smooth progress of the reaction and avoid adverse effects on the reaction caused by too much or too little alkali solution.

[0018] Furthermore, in the above step (1), the molar ratio of dibutyltin dichloride to neodecanoic acid is 1:1.05; the excess ratio of the alkali solution is 12%.

[0019] The beneficial effect of the above is that the ratio of 1:1.05 can enable dibutyltin dichloride to react fully, improve the utilization rate of raw materials, and reduce the impact of unreacted raw materials on product quality.

[0020] Furthermore, in the above step (1), the reaction temperature of dibutyltin dichloride and the alkali solution is 30 - 40 °C, and the time is 1 h; the reaction temperature of dibutyltin oxide and neodecanoic acid is 65 °C, and the time is 2 h; the dropping speed of the alkali solution is 2 - 3 drops / s; the reaction temperature for dropping the alkali solution is 65 °C, and the time is 2 h.

[0021] The further beneficial effects of adopting the above are as follows. A large number of experiments show that the reaction rate at 65°C is moderate, which can not only ensure the efficient progress of the reaction but also avoid side reactions caused by too high temperature, thereby improving the product yield and quality. The reaction time of 2 h can make the reaction sufficient with a high conversion rate, and at the same time, it can avoid the decomposition of the product or other side reactions due to too long reaction time.

[0022] Further, in the above step (2), the washing reagent is deionized water and the number of times is not less than 3 times.

[0023] The further beneficial effects of adopting the above are as follows. When washing, deionized water is used for multiple washes to remove impurities and residual lye.

[0024] Further, in the above step (2), the rotation speed of centrifugal dehydration is 5000 - 6000 r / min and the time is 10 - 20 min.

[0025] The further beneficial effects of adopting the above are as follows. Centrifugal dehydration can effectively remove moisture and improve the product purity.

[0026] Further, in the above step (2), the drying method is vacuum drying, the temperature is 40 - 60°C, and the time is 2 - 4 h.

[0027] The further beneficial effects of adopting the above are as follows. Vacuum drying method is adopted for drying, which is carried out at a lower temperature to prevent the product from thermal decomposition.

[0028] Further, in the above step (2), the precision of the filter for filtration is 0.1 - 0.3 μm.

[0029] The further beneficial effects of adopting the above are as follows. By filtration, insoluble impurities are removed, thus obtaining a high-purity dibutyl-dineodecanoate tin product.

[0030] From the above technical solutions, compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] 1. High product quality: Strictly controlling the raw material purity, optimizing the reaction conditions and the fine post-treatment process make the quality of the prepared dibutyl-dineodecanoate tin product stable, and all indicators meet or exceed the industry standards. The tin content is stably between 20.1% - 20.5%, the chlorine content is less than 0.1%, the moisture content is less than 0.7%, the density and refractive index meet the expectations, and the product appearance is good.

[0032] 2. Yield improvement: The optimized reaction conditions improve the reaction conversion rate, and the direct tin yield reaches more than 96%, which is significantly improved compared with the traditional process, improving the raw material utilization rate and reducing the production cost.

[0033] 3. Good process stability: Verified by scale-up and repeated experiments, the preparation process of the present invention has strong stability, which can ensure the consistency of product quality in different batch productions, providing a reliable guarantee for large-scale industrial production.

[0034] 4. Safe and environmentally friendly: Safety and environmental protection factors are fully considered in raw material selection and reaction process. The use of hazardous chemicals is strictly controlled, and corresponding treatment measures are taken for waste gas, waste water and waste residue generated during the reaction, reducing environmental pollution and meeting the requirements of sustainable development.

[0035] 5. Cost reduction: The optimized process reduces raw material waste and side reactions, and decreases energy consumption and material consumption during the production process. The improved product quality and yield also indirectly reduce the production cost, making the product more competitive in the market.

[0036] 6. The present invention realizes the efficient preparation of dibutyl-tin bis(neodecanoate) by optimizing the synthesis process, improving raw material treatment and innovating the reaction process, which can effectively improve product quality and yield, reduce production cost, ensure the safety and environmental friendliness of the production process, and solve the problems of complex process, unstable product quality, high cost and safety and environmental protection in the prior art.

[0037] 7. The advantages of the preparation method of the present invention are remarkable. The product quality is stable, the tin content is between 20.1% - 20.5%, the chlorine content is less than 0.1%, the moisture content is less than 0.7%, and the density and refractive index meet the expectations; the yield is as high as over 96%, far exceeding the traditional process; the process stability is strong, verified by scale-up and repeated experiments, which can ensure the consistency of product quality in different batches; it is safe and environmentally friendly, strictly controlling the use of hazardous chemicals and properly treating the "three wastes"; the cost is reduced, reducing raw material waste, side reactions and energy and material consumption.

[0038] 8. During the whole reaction process of the present invention, reaction conditions such as temperature, time, raw material ratio, catalyst, protective gas, etc. are precisely controlled, and reasonable post-treatment is carried out after the reaction to ensure product quality. By precisely controlling the reaction conditions, the preparation method of the present invention can significantly improve the product yield of dibutyl-tin bis(neodecanoate), and the yield can reach over 96%. At the same time, the product purity can reach over 95%, which is better than the existing synthesis methods. In addition, the reaction process is relatively stable and easy to operate, which is beneficial to industrial production.

[0039] 9. The dibutyl-tin bis(neodecanoate) prepared by the preparation method of the present invention can be widely applied in the field of PVC heat stability, as well as in polyurethane cross-linking reaction and silanol condensation reaction, strongly promoting the development of related industries. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 is the process flow chart of the preparation method (synthesis route 1) of dibutyl-tin bis(neodecanoate) of the present invention;

[0041] Figure 2 This is the process flow diagram of the preparation method (synthesis route two) of dibutyl-tin dinovate in the present invention. Detailed implementation manners

[0042] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Apparently, the described embodiments are only a part of the embodiments of the present invention, rather than all of them. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without any creative work belong to the scope of protection of the present invention.

[0043] Example 1

[0044] The preparation method (synthesis route one) of dibutyl-tin dinovate is as Figure 1 shown, and specifically includes the following steps:

[0045] (1) Prepare raw materials

[0046] Accurately weigh 100 g of dibutyltin dichloride with a purity of 99.5% and 120 g of neodecanoic acid with a purity of 98.5%, an impurity content of 0.1%, and an acidity value of 324. Prepare 368.5 mL of sodium hydroxide solution with a concentration of 2 mol / L, which contains 29.5 g of sodium hydroxide;

[0047] (2) Synthesize dibutyltin oxide

[0048] Add the sodium hydroxide solution to a reaction kettle equipped with a stirring device, start stirring, slowly add dibutyltin dichloride to the sodium hydroxide solution, react at 30 °C for 1 h, filter after the reaction is completed, and wash the filter cake 3 times with deionized water to obtain dibutyltin oxide;

[0049] (3) Synthesize dibutyl-tin dinovate

[0050] Add dibutyltin oxide to another reaction kettle, then add neodecanoic acid, react at 65 °C for 2 h, and continuously stir during the reaction to make the reaction proceed fully to obtain a crude product;

[0051] (4) Post-treatment of the product

[0052] Transfer the crude product to a separatory funnel, wash it 3 times with deionized water, with 50 mL of water used each time; then perform centrifugal dehydration at a speed of 5000 r / min for 15 min; then, put the dehydrated product into a vacuum drying oven and dry it at 50 °C for 3 h; finally, filter it through a 0.2-μm filter to obtain the dibutyl-tin dinovate product.

[0053] Example 2

[0054] Preparation method of dibutyl-tin dinovate (Synthesis Route 1), as Figure 1 shown, specifically including the following steps:

[0055] (1) Prepare raw materials

[0056] Accurately weigh 120 g of dibutyltin dichloride with a purity of 99.4% and 145 g of novanoic acid with a purity of 98.4%, an impurity content of 0.1%, and an acidity of 326. Prepare 442.5 mL of sodium hydroxide solution with a concentration of 2 mol / L, containing 35.5 g of sodium hydroxide;

[0057] (2) Synthesize dibutyltin oxide

[0058] Add the sodium hydroxide solution to a reaction kettle equipped with a stirring device, start stirring, slowly add dibutyltin dichloride to the sodium hydroxide solution, react at 32 °C for 1 h, filter after the reaction is completed, and wash the filter cake 3 times with deionized water to obtain dibutyltin oxide;

[0059] (3) Synthesize dibutyl-tin dinovate

[0060] Add dibutyltin oxide to another reaction kettle, then add novanoic acid, react at 65 °C for 2 h, and continuously stir during the reaction to make the reaction proceed fully to obtain a crude product;

[0061] (4) Post-treatment of the product

[0062] Transfer the crude product to a separating funnel, wash it 3 times with deionized water, with 50 mL of water used each time; then perform centrifugal dehydration at a rotation speed of 5200 r / min for 14 min; then, put the dehydrated product into a vacuum drying oven and dry it at 52 °C for 3 h; finally, filter it through a 0.2 μm filter to obtain the dibutyl-tin dinovate product.

[0063] Example 3

[0064] Preparation method of dibutyl-tin dinovate (Synthesis Route 2), as Figure 2 shown, specifically including the following steps:

[0065] (1) Prepare raw materials

[0066] Weigh 150 g of dibutyltin dichloride with a purity of 99.2% and 185 g of novanoic acid with a purity of 98.3%, an impurity content of 0.1%, and an acidity of 323. Prepare 553.3 mL of potassium hydroxide solution with a concentration of 2 mol / L, containing 61.97 g of potassium hydroxide;

[0067] (2) Mixing

[0068] Add dibutyltin dichloride and neodecanoic acid to a mixing kettle, stir evenly to obtain a mixed solution;

[0069] (3) Synthesize dibutyl-di-neodecanoate tin

[0070] Transfer the mixed solution to a reaction kettle, slowly dropwise add potassium hydroxide solution at a rate of 2 drops / s, and react at 65 °C for 2 h to obtain a crude product;

[0071] (4) Post-treatment of the product

[0072] Transfer the crude product to a separatory funnel, wash it 3 times with deionized water, with 50 mL of water used each time; then carry out centrifugal dehydration at a speed of 5000 r / min for 15 min; then, put the dehydrated product into a vacuum drying oven and dry it at 50 °C for 3 h; finally, filter it through a 0.2 μm filter to obtain the dibutyl-di-neodecanoate tin product.

[0073] Example 4

[0074] The preparation method of dibutyl-di-neodecanoate tin (Synthesis Route 2), as Figure 2 shown, specifically includes the following steps:

[0075] (1) Prepare raw materials

[0076] Weigh 80 g of dibutyltin dichloride with a purity of 99.6% and 98 g of neodecanoic acid with a purity of 98.6%, an impurity content of 0.1%, and an acidity of 324, and prepare 294.56 mL of potassium hydroxide solution with a concentration of 2 mol / L, which contains 32.99 g of potassium hydroxide;

[0077] (2) Mixing

[0078] Add dibutyltin dichloride and neodecanoic acid to a mixing kettle, stir evenly to obtain a mixed solution;

[0079] (3) Synthesize dibutyl-di-neodecanoate tin

[0080] Transfer the mixed solution to a reaction kettle, slowly dropwise add potassium hydroxide solution at a rate of 3 drops / s, and react at 65 °C for 2 h to obtain a crude product;

[0081] (4) Post-treatment of the product

[0082] Transfer the crude product to a separatory funnel, wash it 3 times with deionized water, with 40 mL of water used each time; then carry out centrifugal dehydration at a speed of 4800 r / min for 12 min; then, put the dehydrated product into a vacuum drying oven and dry it at 45 °C for 2.5 h; finally, filter it through a 0.15 μm filter to obtain the dibutyl-di-neodecanoate tin product.

[0083] Performance Test

[0084] I. Product Characterization

[0085] Take the dibutyl - di - neodecanoate tin products prepared in Examples 1 - 4 respectively, and detect their tin content, chlorine content, moisture content, density, refractive index, chromaticity, appearance, yield and purity. The results are shown in Table 1.

[0086] Table 1 Characterization of Dibutyl - Di - neodecanoate Tin Products in Examples 1 - 4

[0087]

[0088] As can be seen from Table 1, the preparation method of the present invention has significant advantages, the product quality is stable, the tin content is between 20.1% - 20.5%, the chlorine content is less than 0.1%, the moisture content is less than 0.7%, the density and refractive index meet the expectations; the yield is as high as over 96%, and at the same time the product purity can reach over 95%, far exceeding the traditional process.

[0089] II. PVC Thermal Stability Test

[0090] 1. Test Steps:

[0091] (1) Prepare samples: Select commercially available ordinary PVC resin, the dibutyl - di - neodecanoate tin product prepared in Example 2 of the present invention, and a commercially available traditional PVC heat stabilizer as a control.

[0092] (2) Sample preparation: Mix the commercially available ordinary PVC resin with the dibutyl - di - neodecanoate tin product and the commercially available traditional PVC heat stabilizer in certain proportions. Among them, the addition amounts of the dibutyl - di - neodecanoate tin product are set at three gradients of 0.5%, 1.0%, and 1.5%, and 1.2 parts of the commercially available traditional PVC heat stabilizer are added. At the same time, a blank control group without adding a heat stabilizer is set. Stir each mixture evenly in a high - speed mixer.

[0093] (3) Thermal stability test: Use a thermal aging oven to conduct a thermal stability test on the mixed samples. Place the samples in a thermal aging oven at 180°C, take out the samples every 5 minutes to observe the color change, and record the time when the samples start to change color (turn yellow or black).

[0094] 2. Test Data:

[0095] (1) For the blank control group PVC sample without adding a heat stabilizer, at 180°C, it started to turn significantly yellow after 15 minutes, and the color deepened after 30 minutes, with black spots appearing.

[0096] (2) For the PVC sample added with the commercially available traditional PVC heat stabilizer, at 180°C, it started to turn yellow after 40 minutes, and the color was darker after 60 minutes.

[0097] (3) For the PVC sample with 0.5% dibutyl-dineodecanoate tin product added, slight yellowing signs began to appear after 50 min at 180 °C; for the PVC sample with 1.0% dibutyl-dineodecanoate tin product added, it started to turn yellow after 65 min at 180 °C; for the PVC sample with 1.5% dibutyl-dineodecanoate tin product added, slight discoloration occurred after 75 min at 180 °C.

[0098] The above tests show that the dibutyl-dineodecanoate tin product of the present invention can effectively extend the thermal stability time of PVC, and with the increase of the addition amount, the thermal stability effect is more significant.

[0099] III. Polyurethane cross-linking reaction test

[0100] 1. Test steps:

[0101] (1) Raw material preparation: Prepare polyether polyol, isocyanate, the dibutyl-dineodecanoate tin product prepared in Example 2 of the present invention, and a commercially available traditional polyurethane cross-linking reaction catalyst as a control.

[0102] (2) Reaction process: In a dry reaction vessel, first add 10% polyether polyol, and then add 0.8 - 1.2 parts of isocyanate. Divide the reaction system into three groups. One group adds the dibutyl-dineodecanoate tin product with an addition amount of 0.2% of the total mass of the reactants; one group adds a commercially available traditional polyurethane cross-linking reaction catalyst as a control with an addition amount of 0.2% of the total mass of the reactants; one group is a blank control group without adding a catalyst. Seal the reaction vessel and stir the reaction at 50 °C, and observe the viscosity change of the reaction system.

[0103] (3) Performance test: After the reaction is completed, make the prepared polyurethane material into a standard specimen and test its performance indexes such as tensile strength and hardness.

[0104] 2. Test data:

[0105] (1) The reaction in the blank control group was slow, and the viscosity of the system was still low after 12 h of reaction, and it was not completely cross-linked and cured.

[0106] (2) In the experimental group with a commercially available traditional polyurethane cross-linking reaction catalyst added, the viscosity of the system increased significantly after 8 h of reaction, and the cross-linking and curing were basically completed in 10 h. The tensile strength of the prepared polyurethane material was 3 MPa, and the hardness was Shore A60.

[0107] (3) In the experimental group with the dibutyl-dineodecanoate tin product added, the viscosity of the system increased rapidly after 6 h of reaction, and the cross-linking and curing were completed in 8 h. The tensile strength of the prepared polyurethane material reached 3.5 MPa, and the hardness was Shore A65.

[0108] The above tests show that the dibutyl-tin bis(neodecanoate) product of the present invention can effectively accelerate the reaction rate in the polyurethane cross-linking reaction, and the properties of the prepared polyurethane material are better.

[0109] IV. Silanol Condensation Reaction Test

[0110] 1. Test procedure:

[0111] (1) Raw material preparation: Prepare silicone rubber containing silanol groups, cross-linking agent (tetraethyl orthosilicate), the dibutyl-tin bis(neodecanoate) product prepared in Example 2 of the present invention, and a commercially available traditional catalyst for silanol condensation reaction as a control.

[0112] (2) Reaction process: In a clean reaction vessel, mix the silicone rubber and the cross-linking agent (tetraethyl orthosilicate) evenly at ratios of 100:0.5, 100:1, and 100:3 respectively, and divide them into three groups. Add the dibutyl-tin bis(neodecanoate) product to one group, with an addition amount of 0.3% of the mass of the silicone rubber; add a commercially available traditional catalyst for silanol condensation reaction as a control to one group, with an addition amount of 0.3% of the mass of the silicone rubber; and one group serves as a blank control group without adding a catalyst. Seal the reaction vessel and place it at room temperature (25°C), and observe the curing situation of the silicone rubber.

[0113] (3) Performance testing: After curing is completed, perform performance tests on the silicone rubber samples, such as hardness, tensile strength, and tear strength.

[0114] 2. Test data:

[0115] (1) After being placed at room temperature for 72 hours, the blank control group was still not completely cured, and the silicone rubber was in a soft rubber state with no obvious strength.

[0116] (2) In the experimental group adding a commercially available traditional catalyst for silanol condensation reaction, curing started after 24 hours at room temperature and was basically completely cured after 48 hours. The hardness of the cured silicone rubber was Shore A45, the tensile strength was 2 MPa, and the tear strength was 5 kN / m.

[0117] (3) In the experimental group adding the dibutyl-tin bis(neodecanoate) product, curing started after 18 hours at room temperature and was completely cured after 36 hours. The hardness of the cured silicone rubber was Shore A50, the tensile strength was 2.5 MPa, and the tear strength was 6 kN / m.

[0118] The above tests show that the dibutyl-tin bis(neodecanoate) product of the present invention can significantly promote the reaction in the silanol condensation reaction, improve the curing rate of the silicone rubber, and the properties of the cured silicone rubber are more excellent.

[0119] The foregoing description of the disclosed embodiments enables those skilled in the art to practice or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A preparation method of dibutyl-tin dinovate, characterized in that, Specifically, it includes the following steps: (1) First, react dibutyltin dichloride with an alkali solution to generate dibutyltin oxide, and then react dibutyltin oxide with neodecanoic acid to obtain a crude product; Or, first mix dibutyltin dichloride with neodecanoic acid, and then dropwise add an alkali solution for reaction to obtain a crude product; (2) Wash the crude product successively, centrifuge for dehydration, dry, and filter to obtain the dibutyl-di-neodecanoate tin product.

2. The preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (1), the purity of the dibutyltin dichloride is not less than 99%.

3. The preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (1), the purity of the neodecanoic acid is not less than 98%, the impurity content is less than 1%, and the acidity value is 320 - 330.

4. A method for preparing dibutyl-tin dinovate according to claim 1, characterized in that, In step (1), the alkali solution is a sodium hydroxide solution or a potassium hydroxide solution with a concentration of 2 mol / L.

5. The preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (1), the molar ratio of the dibutyltin dichloride to the neodecanoic acid is 1:1.05; the excess ratio of the alkali solution is 12%.

6. The preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (1), the reaction temperature of the dibutyltin dichloride with the alkali solution is 30 - 40 °C and the time is 1 h; the reaction temperature of the dibutyltin oxide with the neodecanoic acid is 65 °C and the time is 2 h; the dropping rate of the alkali solution is 2 - 3 drops / s; the reaction temperature for dropping the alkali solution is 65 °C and the time is 2 h.

7. A preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (2), the washing reagent is deionized water and the number of times is not less than 3 times.

8. A method for preparing dibutyl-tin dinovate according to claim 1, characterized in that, In step (2), the rotation speed for centrifugal dehydration is 5000 - 6000 r / min and the time is 10 - 20 min.

9. A method for preparing dibutyl-tin dinovate according to claim 1, characterized in that, In step (2), the drying method is vacuum drying, the temperature is 40 - 60 °C, and the time is 2 - 4 h.

10. A preparation method of dibutyl-tin dinovate according to claim 1, characterized in that, In step (2), the filter accuracy of the filtration is 0.1 - 0.3 μm.