Preparation method of polyether modified silicone oil for preparing antistatic agent

Abstract

The invention discloses a preparation method of polyether modified silicone oil for preparing an antistatic agent. Comprising the following steps: S1, polyether modified silicone oil raw materials comprise the following components in parts by weight: 100 to 150 parts of high hydrogen-containing silicone oil, 50 to 100 parts of octamethyltetrasiloxane, 50 to 100 parts of hexamethyldisiloxane, 1 to 5 parts of a catalyst, 80 to 100 parts of allyl polyether, 100 to 150 parts of nitrogen, 30 to 50 parts of white oil, 5 to 15 parts of dodecanol and 1 to 5 parts of a polyether activation catalyst; s2, mixing the high-hydrogen-content silicone oil in the S1, octamethyltetrasiloxane, hexamethyldisiloxane and a catalyst, and carrying out a ring-opening polymerization rearrangement reaction under the catalysis of the catalyst to obtain a mixed solution; and S3, filtering the mixed solution in the S2 to obtain the low-hydrogen silicone oil. The polyether modified silicone oil prepared by the invention has the advantages of few impurities and light color, so that the produced polyether modified silicone oil product has high purity and good performance.

Description

Technical Field

[0001] The invention relates to the technical field of polyether modified silicone oil, in particular to a method for preparing polyether modified silicone oil for preparing an antistatic agent. Background Art

[0002] Polyether modified silicone oil is a kind of organic silicon nonionic surfactant with unique properties. It has good lubricity, lower surface tension, better softness and antistatic properties, good leveling properties, can well improve the stress between resin molecules, overcome the shortcomings of these resins themselves, and obtain new properties. It has good demulsification and is suitable for oil-water separation in certain specific occasions. Compared with polydimethylsiloxane, this product can be miscible with water in any proportion, and is also miscible with polar organic solvents such as alcohol, DMF, ether, ester, etc., and partially or completely miscible with non-polar solvents such as toluene and alkanes. It is easy to use and has a wide range of applications; At present, a method for preparing a polyether-modified silicone oil disclosed in a Chinese patent announcement with announcement number CN105504289A comprises: subjecting a terminal olefinic polyether to a hydrosilylation reaction with a hydrogenated silicone oil in a solvent under the action of a porous ceramic-supported platinum catalyst, filtering, and collecting the filtrate; removing the solvent from the filtrate to obtain a polyether-modified silicone oil.

[0003] However, polyether-modified silicone oil can not only be used as a defoaming agent and leveling agent in the industrial field, but is also widely used in daily life, such as textile antistatic agent, cosmetics, etc. The existing polyether-modified silicone oil production process mostly uses simple filtration, activated carbon adsorption and other methods to purify the product. The products produced are prone to residual catalysts, raw materials and other impurities, making them unsuitable for application in daily chemicals and textile antistatic daily life. Therefore, we proposed a preparation method of polyether-modified silicone oil for antistatic agent to solve the above problems. Summary of the invention

[0004] Based on the technical problems existing in the background technology, the present invention proposes a method for preparing polyether-modified silicone oil for preparing antistatic agent.

[0005] The present invention provides a method for preparing a polyether-modified silicone oil for an antistatic agent, comprising the following steps: S1: The polyether-modified silicone oil raw material includes the following components by weight: 100-150 parts of high hydrogen silicone oil, 50-100 parts of octamethyltetrasiloxane, 50-100 parts of hexamethyldisiloxane, 1-5 parts of catalyst, 80-100 parts of allyl polyether, 100-150 parts of nitrogen, 30-50 parts of white oil, 5-15 parts of dodecanol, and 1-5 parts of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 to a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 50-200 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure in S5, and removing unreacted low-boiling point substances by heating; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: passing the semi-finished polyether-modified silicone oil obtained in S7 through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

[0006] Preferably, the catalyst in S1 is a strong acid resin.

[0007] Preferably, the reaction temperature in S2 is 60-70° C., and the reaction time is 6-8 hours.

[0008] Preferably, the stirring speed in S4 is set to 40-60 r / min, and the mixing is performed for 1-2 hours at the stirring speed.

[0009] Preferably, the reaction temperature is 90-100° C. and the reaction time is 3-4 hours.

[0010] Preferably, the temperature in S5 is 80-90° C. and the reaction time is 3-5 h.

[0011] Preferably, the pressure in S6 is set to 100-150 Pa, and the heating temperature is 95-100°C.

[0012] Preferably, sodium hydroxide or sulfuric acid is added to the solution in S6 to adjust the Ph value to 6.5-7.5.

[0013] The polyether-modified silicone oil prepared by the invention has less impurities and light color, so that the produced polyether-modified silicone oil product has high purity and good performance. DETAILED DESCRIPTION

[0014] The present invention will be further explained below in conjunction with specific embodiments. Example

[0015] This embodiment provides a method for preparing a polyether-modified silicone oil for an antistatic agent, comprising the following steps: S1: The polyether-modified silicone oil raw material includes the following components by weight: 100-150 parts of high hydrogen silicone oil, 50 parts of octamethyltetrasiloxane, 50 parts of hexamethyldisiloxane, 1 part of catalyst, 80 parts of allyl polyether, 1000 parts of nitrogen, 30 parts of white oil, 5 parts of dodecanol, and 1 part of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 to a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 50 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure in S5, and removing unreacted low-boiling point substances by heating; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: passing the semi-finished polyether-modified silicone oil obtained in S7 through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

[0016] In this embodiment, the catalyst in S1 is set to a strong acid resin, the reaction temperature in S2 is 60°C, the reaction time is 6 hours, the stirring speed in S4 is set to 40r / min, mixing is carried out at the stirring speed for 12h, the reaction temperature is 90°C, the reaction time is 3h, the temperature in S5 is 80°C, the reaction time is 3h, the pressure in S6 is set to 100 Pa, the heating temperature is 100°C, and sodium hydroxide or sulfuric acid is added to the solution in S6 to adjust the Ph value to 7. Example

[0017] This embodiment provides a method for preparing a polyether-modified silicone oil for an antistatic agent, comprising the following steps: S1: The polyether-modified silicone oil raw material includes the following components by weight: 120 parts of high hydrogen silicone oil, 80 parts of octamethyltetrasiloxane, 70 parts of hexamethyldisiloxane, 3 parts of catalyst, 90 parts of allyl polyether, 130 parts of nitrogen, 40 parts of white oil, 10 parts of dodecanol, and 3 parts of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 to a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 100 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure in S5, and removing unreacted low-boiling point substances by heating; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: passing the semi-finished polyether-modified silicone oil obtained in S7 through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

[0018] In this embodiment, the catalyst in S1 is set to a strong acid resin, the reaction temperature in S2 is 65°C, the reaction time is 7 hours, the stirring speed in S4 is set to 50r / min, mixing is carried out at the stirring speed for 1h, the reaction temperature is 95°C, the reaction time is 3.5h, the temperature in S5 is 85°C, the reaction time is 3h, the pressure in S6 is set to 120 Pa, the heating temperature is 95°C, and sodium hydroxide or sulfuric acid is added to the solution in S6 to adjust the Ph value to 6.5. Example

[0019] This embodiment provides a method for preparing a polyether-modified silicone oil for an antistatic agent, comprising the following steps: S1: The polyether-modified silicone oil raw material includes the following components by weight: 140 parts of high hydrogen silicone oil, 90 parts of octamethyltetrasiloxane, 90 parts of hexamethyldisiloxane, 4 parts of catalyst, 90 parts of allyl polyether, 140 parts of nitrogen, 45 parts of white oil, 13 parts of dodecanol, and 4 parts of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 to a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 180 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure in S5, and removing unreacted low-boiling point substances by heating; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: passing the semi-finished polyether-modified silicone oil obtained in S7 through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

[0020] In this embodiment, the catalyst in S1 is set to a strong acid resin, the reaction temperature in S2 is 70°C, the reaction time is 7 hours, the stirring speed in S4 is set to 60r / min, mixing is carried out at the stirring speed for 1.5h, the reaction temperature is 100°C, the reaction time is 3.5h, the temperature in S5 is 90°C, the reaction time is 4h, the pressure in S6 is set to 150 Pa, the heating temperature is 100°C, and sodium hydroxide or sulfuric acid is added to the solution in S6 to adjust the Ph value to 7.5. Example

[0021] This embodiment provides a method for preparing a polyether-modified silicone oil for an antistatic agent, comprising the following steps: S1: The polyether-modified silicone oil raw material includes the following components by weight: 150 parts of high hydrogen silicone oil, 100 parts of octamethyltetrasiloxane, 100 parts of hexamethyldisiloxane, 5 parts of catalyst, 100 parts of allyl polyether, 150 parts of nitrogen, 50 parts of white oil, 15 parts of dodecanol, and 5 parts of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 into a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 200 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure in S5, and removing unreacted low-boiling point substances by heating; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: passing the semi-finished polyether-modified silicone oil obtained in S7 through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

[0022] In this embodiment, the catalyst in S1 is set to a strong acid resin, the reaction temperature in S2 is 70°C, the reaction time is 8 hours, the stirring speed in S4 is set to 60r / min, and the mixing is carried out at the stirring speed for 2 hours, the reaction temperature is 100°C, and the reaction time is 4 hours, the temperature in S5 is 90°C, and the reaction time is 5 hours, the pressure in S6 is set to 150 Pa, the heating temperature is 100°C, and sodium hydroxide or sulfuric acid is added to the solution in S6 to adjust the Ph value to 7.0.

[0023] The polyether-modified silicone oil prepared by the invention has less impurities and light color, so that the produced polyether-modified silicone oil product has high purity and good performance.

[0024] The polyether-modified silicone oil prepared in the above embodiment is then obtained as a finished product, and after inspection, the data in the following table are obtained:

[0025] The results show that the polyether-modified silicone oil prepared by the present invention is the best embodiment.

[0026] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing polyether-modified silicone oil for antistatic agent, characterized in that: The following steps are involved: S1: The polyether-modified silicone oil raw material includes the following components by weight: 100-150 parts of high hydrogen silicone oil, 50-100 parts of octamethyltetrasiloxane, 50-100 parts of hexamethyldisiloxane, 1-5 parts of catalyst, 80-100 parts of allyl polyether, 100-150 parts of nitrogen, 30-50 parts of white oil, 5-15 parts of dodecanol, and 1-5 parts of polyether activation catalyst; S2: The high hydrogen silicone oil in S1, octamethyltetrasiloxane, hexamethyldisiloxane and the catalyst are mixed, and a ring-opening polymerization rearrangement reaction occurs under the catalysis of the catalyst to obtain a mixed liquid; S3: filtering the mixed liquid in S2 to obtain low hydrogen silicone oil; S4: stirring and mixing the allyl polyether, white oil, dodecanol, and polyether activation catalyst in S1 in a container and reacting them under the action of the catalyst to obtain a polyether solution; S5: adding the low hydrogen silicone oil obtained in S3 and the polyether solution obtained in S4 to a reaction kettle, heating and mixing under a nitrogen environment and a pressure of 50-200 Pa to obtain a preliminary polyether-modified silicone oil solution; S6: maintaining the pressure and heating by increasing the temperature to remove the unreacted low-boiling point substances; S7: filtering the preliminary polyether-modified silicone oil obtained in S5, and adding acid or alkali to adjust the Ph value to neutral, thereby obtaining a semi-finished polyether-modified silicone oil; S8: The semi-finished polyether-modified silicone oil obtained in S7 is passed through a column layer to remove impurities and purify the semi-finished polyether-modified silicone oil, thereby obtaining polyether-modified silicone oil for antistatic agent.

2. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The catalyst in S1 is a strong acid resin.

3. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The reaction temperature in S2 is 60-70° C., and the reaction time is 6-8 hours.

4. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The stirring speed in S4 is set to 40-60 r / min, and mixing is performed for 1-2 hours at the stirring speed.

5. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The reaction temperature is 90-100°C and the reaction time is 3-4h.

6. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The temperature in S5 is 80-90° C. and the reaction time is 3-5 h.

7. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: The pressure in S6 is set to 100-150 Pa, and the heating temperature is 95-100°C.

8. The method for preparing a polyether-modified silicone oil for an antistatic agent according to claim 1, characterized in that: Sodium hydroxide or sulfuric acid is added to the solution in S7 to adjust the Ph value to 6.5-7.5.

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