阅读说明：本技术 一种黏度为475mm2/s～525mm2/s的药用二甲基硅油的生产方法 (Viscosity of 475mm2/s～525mm2Production method of medicinal dimethyl silicone oil/s ) 是由 王祖焕 蔡鹏飞 叶世春 于 2020-05-13 设计创作，主要内容包括：本发明所要解决的技术问题在于提供一种黏度为475mm<Sup>2</Sup>/s～525mm<Sup>2</Sup>/s的药用二甲基硅油的生产方法,以八甲基环四硅氧烷(D4)和六甲基二硅醚为原料。强酸性阳离子交换树脂作催化剂生产药用二甲基硅油。本发明所述方法生产工艺简单,不需要高温焙烧,耗时短,适合工业化生产；采用该方法得到的二甲基硅油黏度处于475mm<Sup>2</Sup>/s～525mm<Sup>2</Sup>/s范围内,其他各项质量指标符合2015版《中国药典》的相关标准要求。(The invention aims to solve the technical problem of providing a high-viscosity polyethylene glycol terephthalate (PEG) with the viscosity of 475mm 2 /s～525mm 2 The production method of the medicinal dimethyl silicone oil/s takes octamethylcyclotetrasiloxane (D4) and hexamethyldisiloxane as raw materials. The strong acid cation exchange resin is used as a catalyst for producing the medicinal dimethyl silicone oil. The method has simple production process, does not need high-temperature roasting, has short time consumption and is suitable for industrial production; the viscosity of the dimethyl silicone oil obtained by the method is 475mm 2 /s～525mm 2 In the range of/s, other quality indexes meet the relevant standard requirements of 2015 edition of Chinese pharmacopoeia.)

1. A method for producing medicinal dimethyl silicone oil with viscosity of 475mm 2/s-525 mm2/s is characterized in that: the production raw materials are octamethylcyclotetrasiloxane (D4) and hexamethyldisiloxane as raw materials; the catalyst is strong acid cation exchange resin.

2. The method for producing the medicinal simethicone with the viscosity of 475mm 2/s-525 mm2/s as claimed in claim 1, wherein the method comprises the following steps: the method comprises the following steps:

1) adding octamethylcyclotetrasiloxane and hexamethyldisiloxane in proportion into a reaction kettle;

2) adding strong-acid cation exchange resin according to a proportion;

3) raising the temperature of the reaction kettle to 30-85 ℃ for catalytic reaction for 8-30 hours;

4) and (4) decompressing, filtering and recovering the catalyst to obtain the simethicone product.

3. The viscosity of claim 2 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: step 1) said octamethyl groupThe mass ratio of the cyclotetrasiloxane to the hexamethyldisiloxane is 100: 1.20-1.50.

4. The viscosity of claim 3 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: the mass ratio of the octamethylcyclotetrasiloxane to the hexamethyldisiloxane is 100: 1.30 to 1.40.

5. The viscosity of claim 2 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: the mass ratio of the strong-acid cation exchange resin to the resin octamethylcyclotetrasiloxane is 3.0-15.0: 100.

6. The viscosity of claim 5 is 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: the mass ratio of the strong-acid cation exchange resin to the resin octamethylcyclotetrasiloxane is 4.0-8.0: 100.

7. The viscosity of claim 6 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: in the step 4), the reduced pressure distillation is carried out for 8-48 hours at the temperature of 160-230 ℃ and under the pressure of ≦ 0.085 MPa.

8. The viscosity of claim 7 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: the reduced pressure distillation temperature is 180-210 ℃.

9. The viscosity of claim 1 of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s is characterized in that: the strong acid cation exchange resin is selected from one of NKC-9 type or HND-34 type.

Technical Field

The invention belongs to the field of pharmaceutical chemistry, and particularly relates to 475mm²/s～525mm²A preparation method of medicinal dimethyl silicone oil with a viscosity range per second.

Technical Field

Dimethicone (Dimethicone), a polydimethylsiloxane having the CAS number 9006-65-9 and the following structural formula:

the simethicone has wide application and can be used as raw and auxiliary materials in the field of medicaments. The simethicone as the auxiliary material is widely applied to each link of preparation production, such as acid-resistant capsules, polishing agents, coating materials, condensing agents, antistatic agents and the like. When the medicinal simethicone is used as a raw material medicament, the pharmacological effects of the medicinal simethicone are mainly defoaming and eliminating vesicular mucus in stomach, and the medicinal simethicone can be prepared into medicinal preparations such as powder, emulsion and the like.

The existing dimethyl silicone oil preparation technology adopts a cyclosiloxane ring-opening polymerization method and a chlorosilane hydrolysis method [ CN12404595A, CN1880361A ], the two methods both need to be catalyzed by acid, the traditional catalyst is concentrated sulfuric acid, and the catalytic reaction is mainly carried out by adopting cation exchange resin after long-term industrial optimization.

Chinese patent CN104231272B adopts acid sulfate as catalyst, and takes octamethylcyclotetrasiloxane (D4 for short) and hexamethyldisiloxane (MM for short) as raw materials to prepare the medicinal dimethyl silicone oil. The viscosity of the produced dimethyl silicone oil is higher than 600mm due to factors such as process conditions, material proportion and the like²(s) viscosity of 475mm which cannot be used in primary grinding of dimethyl silicon oil emulsion²/s～525mm²The viscosity requirement of the dimethyl silicone oil per second.

Chinese patent CN102977370A adopts supported solid super acidic SO₄ ^2-The preparation method of the dimethyl silicone oil comprises the following steps of taking ZrO2-ZSM-5 as a catalyst, and taking octamethylcyclotetrasiloxane (D4 for short) and hexamethyldisiloxane (MM for short) as raw materials to prepare the dimethyl silicone oil. Solid super acidic SO as catalyst in process₄ ^2-The preparation of the/ZrO 2-ZSM-5 is complicated, needs high-temperature roasting, consumes long time and is not suitable for industrial production. The viscosity of the prepared dimethyl silicone oil is lower than 450mm²(s) viscosity of 475mm which cannot be used in primary grinding of dimethyl silicon oil emulsion²/s～525mm²The viscosity requirement of the dimethyl silicone oil per second.

Disclosure of Invention

Aiming at the problem that the viscosity of the raw grinding medicine of the simethicone-free oil emulsion in the existing market is 475mm²/s～525mm²Medicinal dimethyl silicone oil/s. The invention aims to solve the technical problem of providing a high-viscosity polyethylene glycol terephthalate (PEG) with the viscosity of 475mm²/s～525mm²The production method of the medicinal dimethyl silicone oil/s takes octamethylcyclotetrasiloxane (D4) and hexamethyldisiloxane as raw materials. Strong acid cation exchange resinIt is used as catalyst for preparing medicinal dimethyl silicone oil. The method comprises the following specific implementation steps:

1) uniformly mixing octamethylcyclotetrasiloxane (D4) and hexamethyldisiloxane (MM) in a mass ratio of 100: 1.20-1.50 in a reaction kettle, preferably 100: 1.30 to 1.40;

2) adding strong acid cation exchange resin accounting for 3.0-15.0% of the weight of the octamethylcyclotetrasiloxane (D4), wherein the feeding proportion is preferably 4.0-8.0%;

3) raising the temperature to 30-85 ℃ for catalytic reaction for 8-30 hours, preferably 50-65 ℃, and reacting for 22-30 hours;

4) after the reaction is finished, recovering the catalyst by vacuum filtration, and distilling the filtrate at 160-230 ℃ under reduced pressure of ≦ 0.085MPa for 8-48 hours to obtain the simethicone product, wherein the preferred reduced pressure distillation temperature is 180-210 ℃.

2. The strong-acid cation exchange resin is selected from the following types: NKC-9 type, HND-34 type.

The beneficial technical effects of the invention are as follows: the method has simple production process, does not need high-temperature roasting, has short time consumption and is suitable for industrial production; the viscosity of the dimethyl silicone oil obtained by the method is 475mm²/s～525mm²In the range of/s, other quality indexes meet the relevant standard requirements of 2015 edition of Chinese pharmacopoeia.

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