Preparation method of butylbutyl phthalyl glycolate_Kain Industrial Additive

Background and overview^[1]

Butyl phthalyl glycolate is an ester derivative and can be used as a pharmaceutical synthesis intermediate.

Structure

Preparation method^[1-2]

Application examples of butyl phthalyl butyl glycolate are as follows:

1) Prepare a pharmaceutical composition to improve the safety of compound saffron injection. The pharmaceutical composition is mainly made of saffron extract, Ilex polyphylla extract, Fangji extract and butyl butyl phthalyl glycolate. Pharmaceutical compositions for injection. The present invention uses a co-solvent with better safety and more obvious dissolving effect to replace the co-solvent polysorbate 80, which has safety risks and affects product quality in the compound saffron injection, and the safety ratio of butyl butyl phthalyl glycolate Polysorbate 80 is high and the dosage is lower, which reduces the probability and risk of adverse drug reactions and improves the safety of clinical medication.

2) Prepare a manganese-zinc ferrite magnetic sheet for wireless charging. The manganese-zinc ferrite raw material oxides are mixed, pre-burned, and ground to obtain the manganese-zinc ferrite powder with the required performance. The ferrite powder is then processed through pulping, casting, cutting, sintering, laminating, rolling, testing and other processes to obtain manganese-zinc ferrite thin magnetic sheet products, which specifically include the following steps: S1, will include 67 Main component raw materials of ~72wt% Fe 2 O 3 , 22 ~ 27wt% Mn 3 O 4 and 3 ~ 9wt% ZnO, including Nb 2 O 5 , SnO 2 and Co 3 O 4 with a total added amount of less than or equal to 6000ppm. , TiO 2 , ZrO 2 , and CaO, the doping component raw materials of at least one of them are ground, pre-burned, and ground twice to obtain manganese-zinc ferrite powder; S2. The manganese-zinc ferrite powder is mixed with organic matter The slurry is obtained by mixing; S3. The slurry is cast to obtain a cast green sheet; S4. The cast green sheet is sintered to obtain a manganese-zinc ferrite magnetic sheet;

S5. After both sides of the sintered manganese-zinc ferrite magnet sheet are covered with single-sided tape/double-sided tape, the manganese-zinc ferrite magnet sheet for wireless charging is then rolled and crushed to obtain the manganese-zinc ferrite magnet sheet. Preferably, in step S1, the main component raw material and the doping component raw material are uniformly mixed after one ball milling or sanding. The laser particle size of the mixed raw materials after one ball milling or sanding is D50 ≤ 1 μm; The powder is then dried and sieved and then pre-sintered. The pre-sintering temperature is 900~1050℃, the pre-sintering time is 1~5h, and the pre-sintering atmosphere is air sintering. After pre-sintering, the powder is ball milled or sanded twice. After secondary ball milling or sand grinding, the raw materials are mixed with laser particle size D50 = 1~2 μm; after secondary ball milling/sand grinding, the powder is dried and sieved to obtain the required manganese-zinc ferrite powder; the primary ball milling or sand grinding and The grinding media of the secondary ball milling or sanding are all iron balls or zirconia balls. The particle size of the grinding media of the primary ball milling or sanding is D50 = 0.8 ~ 10 μm. The particle size of the grinding media of the secondary ball milling or sanding is D50≤1～10μm; The drying method is spray drying or oven drying.

Preferably, in step S2, the manganese-zinc ferrite powder is mixed with a solvent and a dispersant in a certain proportion, and the mixed slurry is put into a ball mill or sand mill for wetting and dispersion (if If a ball mill is used, the ball mill rotates at a speed of 10-30r/min and disperses for 4 hours; if a sand mill rotates at a speed of 600-1000r/min and disperses for 1 hour (but the invention is not limited to this), the dispersed slurry is Add plasticizer, leveling agent and defoaming agent into the material for grinding (if a ball mill is used, the ball mill speed is 10~30r/min, grinding for 20~40h; if a sand mill is used, the speed is 600~1000r/ min, grinding for 3 to 10 hours, but the invention is not limited thereto), the viscosity of the ground slurry obtained after filtering through metal mesh and defoaming is controlled at 1,000 to 10,000 cP. Preferably, in step S2, based on the manganese-zinc ferrite powder, the solvent content is 30-60wt%, the binder content is 3-10wt%, the plasticizer content is 1-7wt%, and the dispersion The content of agent is 0.2~5wt%, the content of leveling agent is 0.1~1wt%, and the content of defoaming agent is 0.1~1wt%. The dispersant is selected from at least one of oleic acid, linoleic acid or citric acid; preferably, the plasticizer is selected from dioctyl phthalate, dibutyl phthalate, phthalate Dimethyl formate, dibutyl phthalate, butyl stearate, phthalate�At least one of benzyl n-butyl dicarboxylate, butyl butyl phthaloyl glycolate, polyethylene glycol, phthalates, triethyl citrate, methyl acetate, and sodium carboxymethylcellulose A sort of.

Main reference materials

[1] (CN108766705) A manganese-zinc ferrite magnetic sheet for wireless charging and its preparation method

[2] CN201610968043.8 A method for preparing a pharmaceutical composition that improves the safety of compound saffron injection