阅读说明：本技术 一种耐高温碱型氨基硅油乳液的制作方法 (Preparation method of high-temperature-resistant alkali-type amino silicone oil emulsion ) 是由 宋丰伟 于 2019-11-07 设计创作，主要内容包括：本发明属于氨基硅油领域,公开了一种耐高温碱型氨基硅油乳液的制作方法,包括以下步骤：S1：准备好氨基硅油40-50份、乳化剂10-20份、去离子水35-40份、丙三醇添加剂5-10份、三氟甲基马来酸酐3-6份,待用；S2：在高剪切乳化釜中加入乳化剂,开始搅拌。本发明中的三氟甲基马来酸酐可以与氨基硅油发生酰胺化,使氨基硅油结构中的氨基活泼氢减少和增加了羧基,从而达到降低乳液黄变的作用,并且增加氨基硅油乳液的耐高温性和耐碱性,同时乳化剂能够改善乳浊液中各种构成相之间的表面张力,使之形成均匀稳定的分散体系或乳浊液的物质,使氨基硅油乳液具有优异的稳定性,解决了传统氨基硅油乳液易黄变、易破乳和耐高温、耐碱性能差的问题。(The invention belongs to the field of amino silicone oil, and discloses a method for preparing high-temperature alkali-resistant amino silicone oil emulsion, which comprises the following steps: s1: preparing 40-50 parts of amino silicone oil, 10-20 parts of emulsifier, 35-40 parts of deionized water, 5-10 parts of glycerol additive and 3-6 parts of trifluoromethyl maleic anhydride for later use; s2: the emulsifier was added to the high shear emulsification kettle and stirring was started. The trifluoromethyl maleic anhydride can be amidated with amino silicone oil, so that amino active hydrogen in the amino silicone oil structure is reduced and carboxyl is increased, the yellowing effect of the emulsion is reduced, the high temperature resistance and alkali resistance of the amino silicone oil emulsion are increased, meanwhile, the surface tension among various constituent phases in the emulsion can be improved by the emulsifier, and the emulsion can form a uniform and stable dispersion system or an emulsion substance, so that the amino silicone oil emulsion has excellent stability, and the problems of easy yellowing, easy emulsion breaking, and poor high temperature resistance and alkali resistance of the traditional amino silicone oil emulsion are solved.)

1. A method for preparing high-temperature-resistant alkali type amino silicone oil emulsion is characterized in that: the method comprises the following steps:

s1: preparing 40-50 parts of amino silicone oil, 10-20 parts of emulsifier, 35-40 parts of deionized water, 5-10 parts of glycerol additive and 3-6 parts of trifluoromethyl maleic anhydride for later use;

s2: adding an emulsifier into the high-shear emulsifying kettle, and starting stirring;

s3: slowly adding amino silicone oil, stirring for 15-25min, and performing high-speed shearing emulsification;

s4: sequentially adding a glycerol additive and trifluoromethyl maleic anhydride, and adding deionized water while stirring, wherein the water addition amount is 10-20% of the total amount;

s5: adding 1-5 parts of triethylamine, stirring, carrying out system phase inversion, slowly adding the residual ionized water, stirring while adding, adding a pH regulator to adjust the pH to 6-7, and obtaining the high-temperature alkali-resistant amino silicone oil emulsion.

2. The method for preparing the high-temperature-resistant alkali-type amino silicone oil emulsion according to claim 1, wherein the method comprises the following steps: the emulsifier comprises the following raw materials in percentage by mass: ethylene vinyl acetate copolymer, glycol ether: dicetyl diphenyl ether disulfonic acid sodium salt: calcium carbonate: carbon nanotube: water: 1-4:1-4:1-1.5:0.1-0.5:0.1-0.2:4-6.

3. The method for preparing the high-temperature-resistant alkali-type amino silicone oil emulsion according to claim 1, wherein the method comprises the following steps: the preparation method of the emulsifier comprises the following steps: mixing the ethylene-vinyl acetate copolymer, glycol ether, sodium dicetyl diphenyl ether disulfonate, calcium carbonate, carbon nano tubes and water in a container, heating, and stirring for 0.5-1h to obtain the emulsifier.

4. The method for preparing the high-temperature-resistant alkali-type amino silicone oil emulsion according to claim 1, wherein the method comprises the following steps: the pH regulator is aqueous solution of acetic acid and sodium hydrogen phosphate.

5. The method for preparing the high-temperature-resistant alkali-type amino silicone oil emulsion according to claim 1, wherein the method comprises the following steps: the amino silicone oil is prepared by mixing 60% of amino silicone oil with the viscosity of 3500mPa.s and 40% of amino silicone oil with the viscosity of 15000 mPa.s.

Technical Field

The invention relates to the technical field of amino silicone oil emulsion, in particular to a method for preparing high-temperature-resistant alkali type amino silicone oil emulsion.

Background

The silicone oil is colorless, tasteless, nontoxic and non-irritant liquid, and has the characteristics of good chemical stability, heat resistance, cold resistance, weather resistance, hydrophobicity, lubricity, high refractive index, low surface tension and the like. The silicone oil emulsion prepared by emulsifying the silicone oil can be widely used for personal washing and caring articles, textiles and surface treatment.

The amino in the amino silicone oil can interact with hydroxyl, carboxyl and the like on the surface of the fiber, and the amino silicone oil is firmly adsorbed on the fiber, so that the water washing resistance of the fabric is improved; the amino silicone oil forms a film on the surface of the fabric, generally, the larger the molecular weight of the amino silicone oil is, the better the film forming property on the fabric is, the softer the hand feeling is,

the amino silicone oil emulsion is prepared by the polymerization reaction of amino silicone oil, has better storage stability, strong permeability to fibers, large adsorption capacity on the fibers and good coating property, and can improve the action effect of the amino silicone oil, so the amino silicone oil emulsion becomes the most popular soft after-finishing agent in the textile industry, but the existing amino silicone oil emulsion has poor stability, is easy to generate the phenomena of yellowing and emulsion breaking, and has poor high temperature resistance and alkali resistance.

Disclosure of Invention

Technical problem to be solved

1. Technical problem to be solved

Aiming at the problems in the prior art, the invention aims to provide a preparation method of a high-temperature-resistant alkali-type amino silicone oil emulsion, which has the advantages of difficult yellowing, difficult emulsion breaking, high-temperature resistance and alkali resistance, and solves the problems of poor stability, easy yellowing and emulsion breaking of the existing amino silicone oil emulsion, and poor high-temperature resistance and alkali resistance.

(II) technical scheme

In order to achieve the purpose, the invention provides the following technical scheme:

a method for preparing high-temperature alkali-resistant amino silicone oil emulsion comprises the following steps:

s1: preparing 40-50 parts of amino silicone oil, 10-20 parts of emulsifier, 35-40 parts of deionized water, 5-10 parts of glycerol additive and 3-6 parts of trifluoromethyl maleic anhydride for later use;

s2: adding an emulsifier into the high-shear emulsifying kettle, and starting stirring;

s3: slowly adding amino silicone oil, stirring for 15-25min, and performing high-speed shearing emulsification;

s4: sequentially adding a glycerol additive and trifluoromethyl maleic anhydride, and adding deionized water while stirring, wherein the water addition amount is 10-20% of the total amount;

s5: adding 1-5 parts of triethylamine, stirring, carrying out system phase inversion, slowly adding the residual ionized water, stirring while adding, adding a pH regulator to adjust the pH to 6-7, and obtaining the high-temperature alkali-resistant amino silicone oil emulsion.

Preferably, the emulsifier comprises the following raw materials in percentage by mass: ethylene vinyl acetate copolymer, glycol ether: dicetyl diphenyl ether disulfonic acid sodium salt: calcium carbonate: carbon nanotube: water: 1-4:1-4:1-1.5:0.1-0.5:0.1-0.2:4-6.

Preferably, the preparation method of the emulsifier comprises the following steps: mixing the ethylene vinyl acetate copolymer, glycol ether, dicetyl diphenyl ether disulfonic acid sodium, calcium carbonate, carbon nano tubes and water in a container, heating, stirring for 0.5-1h to obtain an emulsifier, enabling the emulsified silicone oil to have strong interface stability through the synergistic effect among the ethylene vinyl acetate copolymer, the glycol ether and the carbon nano tubes, enhancing the emulsion stability, not easily forming layering or emulsion breaking due to the influence of factors such as pH value, salt concentration, temperature and oil phase composition of an acceptor system, and having long stabilization time; meanwhile, the amino silicone oil is matched with the ethylene-vinyl acetate copolymer, so that the color depth effect can be improved.

Preferably, the pH regulator is an aqueous solution of acetic acid and sodium hydrogen phosphate, and the pH regulator of the scheme can enable the electrolyte-resistant stability of the amino silicone oil emulsion to be better.

Preferably, the amino silicone oil is prepared by mixing 60% of amino silicone oil with the viscosity of 3500mPa.s and 40% of amino silicone oil with the viscosity of 15000mPa.s, the amino silicone oil adopted by the scheme can adopt commercially available amino silicone oil, and the scheme preferably uses two amino silicone oils with different viscosities to match, so that not only can the phase inversion speed of emulsion be accelerated and the stability of the emulsion be improved, but also a small amount of the amino silicone oil emulsion can be used in a textile post-treatment agent, so that the textile has good smoothness and softness.

(III) advantageous effects

Compared with the prior art, the invention provides a preparation method of the high-temperature alkali-resistant amino silicone oil emulsion, which has the following beneficial effects:

(1) the trifluoromethyl maleic anhydride can be amidated with amino silicone oil, so that amino active hydrogen in the amino silicone oil structure is reduced and carboxyl is increased, the yellowing effect of the emulsion is reduced, the high temperature resistance and alkali resistance of the amino silicone oil emulsion are increased, meanwhile, the surface tension among various constituent phases in the emulsion can be improved by the emulsifier, and the emulsion can form a uniform and stable dispersion system or an emulsion substance, so that the amino silicone oil emulsion has excellent stability, and the problems of easy yellowing, easy emulsion breaking, and poor high temperature resistance and alkali resistance of the traditional amino silicone oil emulsion are solved.

(1) Triethylamine can react with amino silicone oil to increase the content of hydrophilic group-COO-in emulsion, improve the hydrophilicity of amino silicone oil, enhance the intersolubility of amino silicone oil and water, simultaneously can ensure that a prepolymer in the amino silicone oil is dispersed, a hydrophobic molecular chain is curled to form a core, and a large amount of hydrophilic ionic groups are positioned on the surface of particles and face water when a large amount of-COO-^-The negative ions gather the particle surface and attract corresponding positive ions, and after stabilization, a double electric layer can be formed on the particle surface to generate electromotive force, the electromotive force can prevent the particles from approaching each other and condensing, the emulsifying effect of the amino silicone oil is improved, the particle size of the obtained emulsion is small and stable, and the phenomenon of oil floating can not occur.

(13) The synergistic effect among the ethylene-vinyl acetate copolymer, the glycol ether and the carbon nano tube ensures that the emulsified silicone oil has strong interface stability, enhances the emulsion stability, is not easy to be affected by factors such as pH value, salt concentration, temperature, oil phase composition and the like of a receptor system to form layering or emulsion breaking, and has long stabilization time; meanwhile, the amino silicone oil is matched with the ethylene-vinyl acetate copolymer, so that the color depth effect can be improved.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.