A method for synthesizing a titanium complex and its application in silicone sealant

Abstract

The invention discloses a method for synthesizing a titanium complex and its application in an organic silicon sealant. The invention relates to the field of metal organic compound materials, and comprises the following steps: at a relatively low temperature, titanium tetrachloride reacts with tetrahydrofuran to form a tetrahydrofuran titanium transition compound, and then reacts with isopropanol and ethyl acetoacetate relatively smoothly, so as to smoothly obtain the desired titanium complex. The method for synthesizing a titanium complex described in the invention and its application in an organic silicon sealant, when used in the production of demethanol type silicone sealant, the prepared titanium complex has moderate viscosity and good performance, can meet the conventional performance requirements of the manufacturer, and has the same performance as the primary titanium complex synthesized using tetraisopropyl titanate as a raw material. The primary titanium complex is synthesized using titanium tetrachloride as a raw material instead of conventional tetraisopropyl titanate, and the process of synthesizing tetraisopropyl titanate using titanium tetrachloride can be omitted, thereby shortening the synthesis process and improving production efficiency.

Description

Technical Field

[0001] The invention relates to the field of metal organic compound materials, and in particular to a synthesis method of a titanium complex and application of the titanium complex in organic silicon sealant. Background Art

[0002] One-component demethanol type silicone sealant is one of the important branches of silicone materials. This type of material is widely used and has good bonding properties. When used, it absorbs moisture in the air and releases small methanol molecules to undergo cross-linking and curing. After cross-linking and curing, the basic structural unit of silicone sealant is composed of Si-O chain segments, and the side chains are connected to various other organic groups through silicon atoms. The presence of side groups gives silicone sealants many special properties. Therefore, this special composition and molecular structure of silicone products contains both organic groups and inorganic structures, which makes it combine the characteristics of organic matter with the functions of inorganic matter. Therefore, compared with other polymer materials, silicone products have excellent high and low temperature resistance, weather resistance, electrical insulation, biocompatibility, low surface tension and surface energy and other excellent properties.

[0003] Conventional one-component demethanol type silicone sealant is generally composed of several main components such as α, ω-dihydroxy polydimethylsiloxane (referred to as 107 glue), reinforcing filler, crosslinking agent, coupling agent, catalyst, etc., among which titanium complex plays the role of catalyst and also has the role of partial crosslinking agent and coupling agent. It plays a vital role in this type of sealant and has a huge impact on many properties of sealant, such as mechanical properties, bonding properties, storage properties, etc. Commonly used titanium complexes are generally β-diketone substances, such as ethyl acetoacetate, acetylacetone, etc.

[0004] Commonly used titanium complexes can be further reacted with diols to obtain hexacoordinated chelated secondary titanium complexes with lower reaction activity and better stability. It can be seen that the synthesis of primary titanium complexes is very important. Conventional primary titanium complexes are synthesized by transesterification of ethyl acetoacetate and tetraisopropyl titanate. The raw material for synthesizing tetraisopropyl titanate is titanium tetrachloride, which is very easy to react with water vapor and undergoes violent hydrolysis in the air, showing a phenomenon of smoking. The reaction with isopropanol and ethyl acetoacetate is also very violent, releasing a large amount of heat and by-products. The reaction is very difficult to control, and if the HCl produced by the reaction is not neutralized in time, it is easy to degrade ethyl acetoacetate. The overall synthesis control is very difficult, and the desired primary titanium complex is often not obtained in the end. Therefore, the current synthesis route is generally: titanium tetrachloride → tetraisopropyl titanate → primary titanium (→ secondary titanium). That is, titanium tetrachloride reacts with isopropanol in a solvent, hydrogen chloride is neutralized with ammonia, and tetraisopropyl titanate is obtained after the solvent is removed and purified; tetraisopropyl titanate reacts with ethyl acetoacetate to obtain a primary titanium complex. Summary of the invention

[0005] The main purpose of the present invention is to provide a method for synthesizing a titanium complex and its application in organic silicon sealant, which can effectively solve the problems in the background technology.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A method for synthesizing a titanium complex comprises the following steps:

[0008] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the titanium tetrachloride is 190Kg, the ethyl acetoacetate is 260Kg, the isopropanol is 120Kg, the cyclohexane is 380-1140Kg, the tetrahydrofuran is 380-1140Kg, and the actual amount of NH3 shall prevail;

[0009] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0010] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0011] Preferably, the titanium tetrachloride is 190 Kg, ethyl acetoacetate is 260 Kg, isopropanol is 120 Kg, cyclohexane is 380 Kg, tetrahydrofuran is 1140 Kg, and the actual amount of NH3 shall prevail.

[0012] Preferably, the titanium tetrachloride is 190 Kg, ethyl acetoacetate is 260 Kg, isopropanol is 120 Kg, cyclohexane is 570 Kg, tetrahydrofuran is 950 Kg, and the actual amount of NH3 shall prevail.

[0013] Preferably, the titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 760Kg, tetrahydrofuran is 760Kg, and the actual amount of NH3 shall prevail.

[0014] Preferably, the titanium tetrachloride is 190 Kg, ethyl acetoacetate is 260 Kg, isopropanol is 120 Kg, cyclohexane is 950 Kg, tetrahydrofuran is 570 Kg, and the actual amount of NH3 shall prevail.

[0015] Preferably, the titanium tetrachloride is 190 Kg, ethyl acetoacetate is 260 Kg, isopropanol is 120 Kg, cyclohexane is 1140 Kg, tetrahydrofuran is 380 Kg, and the actual amount of NH3 shall prevail.

[0016] Preferably, the molar ratio of titanium tetrachloride, ethyl acetoacetate and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran and cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran and titanium tetrachloride is 5.3:1-10.6:1.

[0017] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] In the present invention, when the prepared titanium complex is used for the production of demethanol type silicone sealant, the viscosity is moderate and the performance is good, which can meet the conventional performance requirements of the manufacturer and is consistent with the performance of the primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. The primary titanium complex is synthesized by using titanium tetrachloride as a raw material instead of conventional tetraisopropyl titanate, so that the process of synthesizing tetraisopropyl titanate with titanium tetrachloride can be omitted, the synthesis process is shortened, and the production efficiency of the primary titanium complex is improved. In the synthesis process, tetrahydrofuran is selected as a solvent and a stabilizer, and the excess tetrahydrofuran is used to have a good coordination ability with titanium tetrachloride, so that the formed transition compound, tetrachlorobis(titanium), reacts stably with β-diketone substances and monohydric alcohols, and the process is controllable, and finally a primary titanium complex with excellent performance is obtained;

[0020] The mixed solvent used in the reaction is tetrahydrofuran-cyclohexane, which has a very good solubility for transition tetrahydrofuran titanium and a low boiling point, and is convenient and simple to post-process. After the reaction is completed and the mixture is pumped out, the composition and weight are almost unchanged, and the mixture can be reused. The obtained ammonium chloride solid is very pure and can be sold directly, thus saving production costs and waste liquid treatment costs. High temperature is not required throughout the reaction, and the solvent can be pumped out cleanly under reduced pressure at about 50° C. The obtained primary titanium complex does not need to be cooled and can be directly discharged, and the synthetic production is safe and efficient.

[0021] The entire synthesis process adopts an in-situ reaction method, which efficiently and quickly completes the reaction that originally needed to be completed in steps, saving resources and energy. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a process diagram of the preparation reaction formula 1 of the present invention;

[0023] Figure 2 It is a process diagram of preparing reaction formula 2 of the present invention. DETAILED DESCRIPTION

[0024] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] like Figure 1-2 As shown, a method for synthesizing a titanium complex comprises the following steps:

[0026] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3. The amount of titanium tetrachloride is 190 kg, the amount of ethyl acetoacetate is 260 kg, the amount of isopropanol is 120 kg, the amount of cyclohexane is 380-1140 kg, the amount of tetrahydrofuran is 380-1140 kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0027] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0028] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0029] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. Specific embodiment one:

[0031] A method for synthesizing a titanium complex comprises the following steps:

[0032] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the amount of titanium tetrachloride is 190 kg, the amount of ethyl acetoacetate is 260 kg, the amount of isopropanol is 120 kg, the amount of cyclohexane is 380 kg, the amount of tetrahydrofuran is 1140 kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0033] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0034] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0035] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. Specific embodiment 2:

[0037] A method for synthesizing a titanium complex comprises the following steps:

[0038] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the amount of titanium tetrachloride is 190Kg, the amount of ethyl acetoacetate is 260Kg, the amount of isopropanol is 120Kg, the amount of cyclohexane is 570Kg, the amount of tetrahydrofuran is 950Kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0039] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0040] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0041] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. Specific embodiment three:

[0043] A method for synthesizing a titanium complex comprises the following steps:

[0044] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the amount of titanium tetrachloride is 190 kg, the amount of ethyl acetoacetate is 260 kg, the amount of isopropanol is 120 kg, the amount of cyclohexane is 760 kg, the amount of tetrahydrofuran is 760 kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0045] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0046] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0047] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. Specific embodiment four:

[0049] A method for synthesizing a titanium complex comprises the following steps:

[0050] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the amount of titanium tetrachloride is 190Kg, the amount of ethyl acetoacetate is 260Kg, the amount of isopropanol is 120Kg, the amount of cyclohexane is 950Kg, the amount of tetrahydrofuran is 570Kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0051] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0052] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0053] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material. Specific embodiment five:

[0055] A method for synthesizing a titanium complex comprises the following steps:

[0056] S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the amount of titanium tetrachloride is 190 kg, the amount of ethyl acetoacetate is 260 kg, the amount of isopropanol is 120 kg, the amount of cyclohexane is 1140 kg, the amount of tetrahydrofuran is 380 kg, and the amount of NH3 is based on the actual amount used. The molar ratio of titanium tetrachloride, ethyl acetoacetate, and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran to cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran to titanium tetrachloride is 5.3:1-10.6:1;

[0057] S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes;

[0058] S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

[0059] The invention discloses an application of a titanium complex in an organic silicon sealant, which is applied to a demethanol type organic silicon sealant and has the same performance as a primary titanium complex synthesized by using tetraisopropyl titanate as a raw material.

[0060] The titanium complexes prepared in specific examples 1 to 5 were compared with comparative example 1. Specific examples 1 to 5 are recorded as examples 1-5, which are diisopropyldititanium with the same structure.

[0061] Preparation of demethanol type silicone sealant:

[0062] The base material composition is as follows: 100 parts of α,ω-dihydroxy polydimethylsiloxane (viscosity: 8000cps); 90 parts of nano calcium carbonate; 30 parts of heavy calcium carbonate;

[0063] Base material preparation method:

[0064] Add all the α,ω-dihydroxypolydimethylsiloxane into a vacuum kneader, then add all the nano calcium carbonate and heavy calcium carbonate under stirring, turn on the heating, and vacuum dehydrate at 135°C and above -0.09MPa for 3 hours. Discharge the obtained base material while hot at 90°C, seal it, and store it in a cooled state.

[0065] Composition and preparation of sealant:

[0066] Base material: 1000 parts; Methyltrimethoxysilane: 32.5 parts; Examples 1-5 and Comparative Example 1: 11 parts each; KH560 coupling agent: 3.5 parts;

[0067] Methyltrimethoxysilane was added to the base material, and the mixture was evenly dispersed by vacuum stirring. Then, the coupling agent in the embodiment and comparative example was evenly mixed and added to the above materials. The mixture was evenly dispersed by vacuum stirring. The discharged materials were sealed and stored to obtain the test products of embodiments 1, 2, 3, 4, 5 and comparative example 1, respectively.

[0068] Performance Test:

[0069] The surface drying time test refers to: GB / T13477.5-2017 Test method for building sealing materials; Shore A hardness test refers to: GB / T531.1-2008 Test method for indentation hardness of vulcanized rubber or thermoplastic rubber; Tensile performance test (maximum strength, maximum strength elongation, bonding failure area) refers to: GB16776-2005 Silicone structural sealant for construction; Storage period test: Indoor conditions, temperature 25±2℃, humidity 55±5%, surface drying time and 24-hour strip curing are tested every 30 days. At the same time, if the surface drying time is ≤60min and the 24-hour strip curing is normal, it is judged to be within the storage period. The following is the test table:

[0070]

[0071] According to the above table, embodiments 1-5 are almost the same as comparative example 1 in terms of surface drying time, hardness, maximum bonding strength, maximum strength elongation, bonding failure area, storage, etc., reaching or exceeding the corresponding national standards. It can be seen that when the primary titanium synthesized by the present invention is used in the production of demethanol type silicone sealant, the product is consistent with the primary titanium synthesized with tetraisopropyl titanate as raw material in terms of performance, and the former can replace the latter. The comprehensive advantages embodied by the present invention are more obvious, and the purpose of the invention has been achieved.

[0072] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for synthesizing a titanium complex, characterized in that: The steps include: S1: Prepare raw materials, including titanium tetrachloride, ethyl acetoacetate, isopropanol, cyclohexane, tetrahydrofuran, and NH3, wherein the titanium tetrachloride is 190Kg, the ethyl acetoacetate is 260Kg, the isopropanol is 120Kg, the cyclohexane is 380-1140Kg, the tetrahydrofuran is 380-1140Kg, and the actual amount of NH3 shall prevail; S2: First, tetrahydrofuran and cyclohexane are mixed uniformly in a reaction kettle according to the required ratio and quantity, and the temperature is controlled not to be higher than 20°C. Then, under the protection of nitrogen, titanium tetrachloride is injected into the mixed solvent formed by tetrahydrofuran and cyclohexane and mixed thoroughly. The temperature during the process does not exceed 25°C. Under rapid stirring, half of the mixed mixture of ethyl acetoacetate and isopropanol is added dropwise to the above materials, and the material temperature is controlled not to be higher than 40°C. The addition is completed within 30 minutes; S3: Immediately and rapidly pass NH3 into the material formed by S2 until a large amount of solid matter appears. Continue to pass NH3 and dropwise add the remaining mixture of ethyl acetoacetate and isopropanol. The addition is completed within 30 minutes. The reaction is determined to be complete when no chlorine element is present in the liquid material. Stop passing NH3. After the material is centrifuged, the resulting liquid part is heated to 50°C. Open the vacuum under stirring and pump out all the solvent. The resulting material is the primary titanium complex, which can be directly discharged and sealed.

2. The method for synthesizing a titanium complex according to claim 1, characterized in that: The titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 380Kg, tetrahydrofuran is 1140Kg, and the actual amount of NH3 shall prevail.

3. The method for synthesizing a titanium complex according to claim 1, characterized in that: The titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 570Kg, tetrahydrofuran is 950Kg, and the actual amount of NH3 shall prevail.

4. The method for synthesizing a titanium complex according to claim 1, characterized in that: The titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 760Kg, tetrahydrofuran is 760Kg, and the actual amount of NH3 shall prevail.

5. The method for synthesizing a titanium complex according to claim 1, characterized in that: The titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 950Kg, tetrahydrofuran is 570Kg, and the actual amount of NH3 shall prevail.

6. The method for synthesizing a titanium complex according to claim 1, characterized in that: The titanium tetrachloride is 190Kg, ethyl acetoacetate is 260Kg, isopropanol is 120Kg, cyclohexane is 1140Kg, tetrahydrofuran is 380Kg, and the actual amount of NH3 shall prevail.

7. The method for synthesizing a titanium complex according to claim 1, characterized in that: The molar ratio of titanium tetrachloride, ethyl acetoacetate and isopropanol is 1:2:2, the weight ratio of tetrahydrofuran and cyclohexane is 3:1-1:3, and the molar ratio of tetrahydrofuran and titanium tetrachloride is 5.3:1-10.6:

1.

8. Use of a titanium complex in an organic silicon sealant, using the synthesis method of a titanium complex according to any one of claims 1 to 7, characterized in that: When used in demethanol type silicone sealant, its performance is consistent with that of the primary titanium complex synthesized using tetraisopropyl titanate as raw material.

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