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Preparation method of ternary block organic-silicon softening agent

A technology of silicone softener and ternary block, which is applied in the direction of textiles, papermaking, fiber treatment, etc., can solve the problems of complicated process and difficult control of solid content, so as to improve the softness of fabrics, increase the lightness and smoothness, increase the The effect of hand feeling

Inactive Publication Date: 2014-12-10
广东科司达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The more advanced product is block silicone oil, that is, the amino polyether chain segment with good hydrophilicity is embedded in the silicone product through block copolymerization, and the above-mentioned problems are solved by using the recessive cationic characteristics of the amino group and the hydrophilicity of the polyether. The existing block silicone oil preparation method needs to prepare and purify the silicone oil intermediate first, the process is complicated, and it is difficult to control the solid content during use

Method used

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  • Preparation method of ternary block organic-silicon softening agent

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preparation example Construction

[0021] The preparation method of the ternary block organosilicon softening agent of the present invention specifically comprises the following steps:

[0022] Step 1: Add 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane (cas number: 126 -80-7) and polyetheramine are added to the reactor according to the ratio of 0.5 to 2:1, and isopropanol is added which is equal to the total mass of the epoxy-terminated agent and polyetheramine, and then the temperature is raised to 70 ℃~100℃ for 3~6 hours to obtain polyether modified end-capping agent;

[0023] Step 2: Cool down the polyether modified end-capping agent obtained in step 1 to 45°C to 55°C, add octamethylcyclotetrasiloxane (D4) which is 25 to 40 times the mass of the end-epoxy end-capping agent, and end-capping agent Epoxy end-capping agent, polyetheramine and octamethylcyclotetrasiloxane catalyst tetramethylammonium hydroxide with a total mass of 0.5‰~1‰, turn on the vacuum pump, adjust the vacuum degree to 0....

Embodiment 1

[0027] Step 1: Mix the end-epoxy blocking agent 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane and polyetheramine ED -2003 According to the material ratio of 1.1:1, add isopropanol into the reactor, and add isopropanol equal to the total mass of epoxy-terminated agent and polyether amine, and then raise the temperature to 85°C for 4 hours to obtain polyether modified blocking agent;

[0028] Step 2: Cool the polyether modified end-capping agent obtained in step 1 to 50°C, add D4, which is 28 times the mass of the epoxy-terminated end-capping agent, and the epoxy-terminated end-capping agent, polyetheramine ED-2003 and octamethyl Catalyst tetramethylammonium hydroxide with a total mass of cyclotetrasiloxane of 0.5‰, turn on the vacuum pump, adjust the vacuum degree to 0.8MPa, raise the temperature to 80°C, vacuum-dry for 1 hour, and simultaneously extract isopropanol, then return to normal pressure, and Cool down to 50°C and then react at 80°C for 5 hours, th...

Embodiment 2

[0031] Step 1: Mix the end-epoxy blocking agent 1,1,3,3-tetramethyl-1,3 bis[3-(oxiranylmethoxy)propyl]disiloxane and polyetheramine ED -2003 According to the material ratio of 0.5:1, add isopropanol into the reactor, and add isopropanol equal to the total mass of epoxy-terminated agent and polyether amine, and then heat up to 70°C for 6 hours to obtain polyether modified blocking agent;

[0032] Step 2: Cool down the polyether modified end-capping agent obtained in step 1 to 55°C, add D4, which is 40 times the mass of the epoxy-terminated end-capping agent, and the epoxy-terminated end-capping agent, polyetheramine ED-2003 and octamethyl Catalyst tetramethylammonium hydroxide with a total mass of cyclotetrasiloxane of 1‰, turn on the vacuum pump, adjust the vacuum degree to 0.6MPa, raise the temperature to 80°C, and vacuum-dry for 1 hour, while extracting isopropanol, then return to normal pressure, and Cool down to 50°C and then react at 110°C for 2 hours, the viscosity of t...

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Abstract

The invention discloses a preparation method of a ternary block organic-silicon softening agent. The preparation method comprises the steps of firstly reacting an end-epoxy end blocking agent and polyether amine to obtain a polyether-modified end blocking agent; then adding octamethylcyclotetrasiloxane and a catalyst for reaction to obtain a ternary block organic-silicon copolymer; and finally adding isopropyl alcohol into the ternary block organic-silicon copolymer till the needed solid content is reached, heating and stirring to obtain the ternary block organic-silicon softening agent. The preparation method disclosed by the invention has the advantages that the mode of firstly preparing a modified end blocking agent and then adding D4 for chain-extending polymerization to obtain the ternary block organic silicon is adopted, the step of preparing silicon-oil intermediate for purification is omitted, the solid content can be effectively controlled, an additional emulsifying agent does not need to be added, the emulsification is easy without oil floating, a product can be used by directly diluting, additional operation is not needed, the production efficiency can be greatly improved, the cost can be effectively reduced, and the softening performance of the fabric can be improved when the ternary block organic-silicon softening agent is applied to softening finish of the fabric.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a preparation method of a three-element block silicone softener. Background technique [0002] Silicone softeners are silicone-based polymers and their derivatives. Its softening effect is that the oxygen atoms in the silicon-oxygen bond are adsorbed on the surface of the fiber, making the hydrophobic methyl group oriented and covering the fiber surface. Since the bond angle of the silicon-oxygen bond can be changed under the action of external force to produce stretching, therefore, the fabric treated with silicone softener forms a tough, water-repellent and stretchable continuous film on the surface of the fabric, which not only makes the fabric soft The smooth performance also endows the surface of the fabric with gloss, elasticity, fullness, anti-wrinkle, wear resistance, anti-fouling and strong wool feeling, and can improve the sewing property of the f...

Claims

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Application Information

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IPC IPC(8): D06M15/647C08G77/46
Inventor 贺江平崔妍蕾闵欣
Owner 广东科司达新材料科技有限公司