Preparation method of biomass tributyl borate

Abstract

The invention discloses a preparation method of biomass tributyl borate, which comprises the following steps: decomposing 1500L of butyl acetate, pouring into a reaction kettle, vacuumizing to obtain a mixed solution a, and removing impurities from the obtained mixed solution a; adding a water-carrying agent and a catalyst into the obtained mixed solution a, and mixing and stirring to obtain a mixed solution b; according to the present invention, the prepared biomass material is subjected to impurity removal treatment, such that the fine particle impurities in the material can be effectively removed, the tributyl borate preparation time is shortened by using the preparation method, the water-carrying agent and the catalyst are easily decomposed from the system so as not to cause the reduction of the purity rate of the obtained material, and the method is suitable for industrial production. And the whole preparation steps conform to specifications, so that the operation risk is greatly reduced, and the use quality and purity of the tributyl borate are ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of tributyl borate, and specifically relates to a method for preparing biomass tributyl borate. Background Art

[0002] Tributyl borate is an intermediate for preparing borohydrides, and can be used for synthesizing semiconductor boron diffusion sources, fire retardants, adhesives and desiccants for anhydrous systems. In addition, it can also be used as a polymer additive, gasoline additive, sterilant, flame retardant, automotive brake fluid and special surfactant, and its application range is very wide. At present, the steps required for preparing biomass tributyl borate are complex, and the obtained biomass tributyl borate contains more impurities, which affects its purity during use. In addition, particles in the obtained material cannot be removed after the distillation reaction, and the reaction time is long during later use, which affects the use quality. Summary of the Invention

[0003] The purpose of the present invention is to provide a method for preparing biomass tributyl borate to solve the problems raised in the above background art.

[0004] To achieve the above purpose, the present invention provides the following technical solution: A method for preparing biomass tributyl borate, and the preparation method includes the following steps:

[0005] S1. Decompose 1500 L of butyl acetate, pour it into a reaction kettle for vacuum treatment to obtain a mixed liquid a, and perform impurity removal treatment on the obtained mixed liquid a;

[0006] S2. Then add a water-carrying agent and a catalyst to the above-obtained mixed liquid a, and perform mixing and stirring to obtain a mixed liquid b;

[0007] S3. Then pour the above-obtained mixed liquid b into a mixing tank for stirring, add boric acid for esterification reaction, and continuously stir to obtain a mixed liquid c;

[0008] S4. Pour the mixed liquid c into a distillation kettle for distillation reaction, and use a filter screen to remove impurities to obtain tributyl borate.

[0009] Preferably, the vacuum pressure in step 1 is between 0.03 MPa and 0.05 MPa.

[0010] Preferably, the capacity of the water-carrying agent added in step 2 is 15%, and the capacity of the catalyst is 10%.

[0011] Preferably, the mixing and stirring speed in step 2 is 80 - 100 rpm / min.

[0012] Preferably, the stirring time for the mixed solution b in step S3 is 25 min, and the esterification reaction time is 20 min.

[0013] Preferably, the biomass material obtained after the distillation reaction is filtered through a sieve mesh with a sieve hole diameter of 0.0450 mm and a mesh number of 325 to remove fine particle impurities, thereby improving the purity of the material.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] 1. By performing impurity removal treatment on the prepared biomass material, the present invention can effectively remove fine particle impurities in the material. Moreover, this preparation method shortens the preparation time of tributyl borate, and the water-carrying agent and catalyst are easily decomposed from the system, which will not cause a decrease in the purity of the obtained material. In addition, the overall preparation steps comply with the specifications, greatly reducing the operation risk and ensuring the use quality and purity of tributyl borate. Specific Embodiments

[0016] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0017] To achieve the above object, the present invention provides the following technical solution: A method for preparing tributyl borate from biomass, the preparation method comprising the following steps:

[0018] S1. Decompose 1500 L of butyl acetate and pour it into a reaction kettle for vacuum treatment to obtain a mixed solution a, and perform impurity removal treatment on the obtained mixed solution a;

[0019] S2. Then add a water-carrying agent and a catalyst to the above-obtained mixed solution a and perform mixing and stirring to obtain a mixed solution b;

[0020] S3. Then pour the above-obtained mixed solution b into a mixing tank for stirring, add boric acid for esterification reaction, and continuously stir to obtain a mixed solution c;

[0021] S4. Pour the mixed solution c into a distillation kettle for distillation reaction, and use a filter screen to remove impurities to obtain tributyl borate.

[0022] Example 1:

[0023] A method for preparing tributyl borate from biomass, the preparation method comprising the following steps:

[0024] S1. Decompose 1500 L of butyl acetate and pour it into a reaction kettle for vacuum treatment. The vacuum pressure is 0.03 MPa to obtain a mixed solution a, and perform impurity removal treatment on the obtained mixed solution a;

[0025] S2. Then add 15% of a water-carrying agent and 10% of a catalyst to the above-obtained mixed solution a, and perform mixing and stirring. The mixing and stirring speed is 80 rpm / min to obtain a mixed solution b;

[0026] S3. Then pour the above-obtained mixed solution b into a mixing tank for stirring. The stirring time is 25 min, and the esterification reaction time is 20 min. Add boric acid for esterification reaction and continue stirring to obtain a mixed solution c;

[0027] S4. Pour the mixed solution c into a distillation kettle for distillation reaction, and use a filter screen to remove impurities to obtain tributyl borate.

[0028] Example 2:

[0029] A method for preparing biomass tributyl borate, the preparation method comprising the following steps:

[0030] S1. Decompose 1600 L of butyl acetate and pour it into a reaction kettle for vacuum treatment. The vacuum pressure is 0.05 MPa to obtain a mixed solution a, and perform impurity removal treatment on the obtained mixed solution a;

[0031] S2. Then add 17% of a water-carrying agent and 15% of a catalyst to the above-obtained mixed solution a, and perform mixing and stirring. The mixing and stirring speed is 100 rpm / min to obtain a mixed solution b;

[0032] S3. Then pour the above-obtained mixed solution b into a mixing tank for stirring. The stirring time is 30 min, and the esterification reaction time is 25 min. Add boric acid for esterification reaction and continue stirring to obtain a mixed solution c;

[0033] S4. Pour the mixed solution c into a distillation kettle for distillation reaction, and use a filter screen to remove impurities to obtain tributyl borate.

[0034] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A preparation method of biomass tributyl borate, characterized in that: The preparation method comprises the following steps: S1. Decompose 1500 L of butyl acetate and pour it into a reaction kettle for vacuum treatment to obtain a mixed solution a, and perform impurity removal treatment on the obtained mixed solution a; S2. Then add a water-carrying agent and a catalyst to the above-obtained mixed solution a and mix and stir to obtain a mixed solution b; S3. Then pour the above-obtained mixed solution b into a mixing tank for stirring, add boric acid for esterification reaction, and continuously stir to obtain a mixed solution c; S4. Pour the mixed solution c into a distillation kettle for distillation reaction, and use a filter screen to remove impurities to obtain tributyl borate.

2. The preparation method of biomass tributyl borate according to claim 1, characterized in that: The vacuum pressure in step 1 is between 0.03 MPa and 0.05 MPa.

3. The preparation method of biomass tributyl borate according to claim 1, characterized in that: The capacity of the water-carrying agent added in step 2 is 15%, and the capacity of the catalyst is 10%.

4. The preparation method of biomass tributyl borate according to claim 1, characterized in that: The mixing and stirring speed in step 2 is 80 - 100 rpm / min.

5. The preparation method of biomass tributyl borate according to claim 1, characterized in that: The stirring time of the mixed solution b in step S3 is 25 min, and the esterification reaction time is 20 min.

6. The preparation method of biomass tributyl borate according to claim 1, characterized in that: The biomass material obtained after the distillation reaction is filtered with a filter screen having a screen hole diameter of 0.0450 mm and a mesh number of 325 meshes to effectively remove fine particle impurities and improve the purity of the material.