Method for preparing fluorine-containing silicon acrylate emulsion

A silicon acrylate and acrylate technology, which is applied in the field of acrylate modification, can solve the problems of fabrics with unpleasant smell of quaternary ammonium salt cationic surfactant residues, difficult biodegradation of fluoroalkanes, and unsatisfactory effects, etc. Industrial application prospect, excellent waterproof and oil-proof performance, and the effect of stable and excellent waterproof and oil-proof performance

Active Publication Date: 2011-07-20
苏州优诺塑业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technical solution has the following obvious deficiencies: one, ① perfluorohexyl ethyl acrylate, ② perfluorooctyl ethyl acrylate, ③ perfluorodecyl ethyl acrylate, ④ perfluorohexyl ethyl acrylate Methacrylate, ⑤ Perfluorooctylethyl methacrylate, ⑥ Perfluorodecylethyl methacrylate and other monomers are currently produced by very few domestic manufacturers, or they are difficult to produce and expensive
In addition, the biodegradation of long-chain fluorinated alkanes is difficult, and the sewage treatment is difficult
Second, the fabrics treated with quaternary ammonium salt cationic surfactants have unpleasant smell of quaternary ammonium salt cationic surfactant residues
3. The water-repellent performance (polyester) of the water-repellent and oil-repellent agent obtained by ...

Method used

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  • Method for preparing fluorine-containing silicon acrylate emulsion
  • Method for preparing fluorine-containing silicon acrylate emulsion
  • Method for preparing fluorine-containing silicon acrylate emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Embodiment one: the preparation process sees figure 2 : Mix 20 grams of octamethylcyclotetrasiloxane, 8 grams of 1,3,5-trimethyl-1,3,5-tris(3,3,3-trifluoropropyl)cyclotrisiloxane, 3 grams of tetramethyltetravinylcyclotetrasiloxane, 15 grams of methyl methacrylate, 35 grams of butyl acrylate, 1.5 grams of TX-10, 3 grams of fluorinated anionic emulsifier, 0.3 grams of APS, 0.6 grams of hydroxide Mix potassium and 120 grams of distilled water for 15 minutes under high shear, take out 1 / 3 of the emulsion and add it to a four-neck round bottom flask, turn on nitrogen protection, heat to 80°C while stirring, and drop the remaining 2 / 3 of the emulsion into the reaction flask within 3 hours , after all the drops were completed, the temperature was raised to 85°C, and the reaction was continued for 3 hours, then stirred and lowered to room temperature, and the discharge was filtered to obtain the target product.

Embodiment 2

[0045] Embodiment two: preparation process see figure 2 : Mix 35 grams of octamethylcyclotetrasiloxane, 8 grams of 1,3,5-trimethyl-1,3,5-tris(3,3,3-trifluoropropyl)cyclotrisiloxane, 5 grams of tetramethyltetravinyl cyclotetrasiloxane, 22.5 grams of methyl methacrylate, 27.5 grams of butyl acrylate, 4.7 grams of TX-10, 4.0 grams of fluorinated anionic emulsifier, 0.5 grams of APS, 0.7 grams of hydroxide Mix potassium and 100 grams of distilled water for 15 minutes under high shear, take out 1 / 3 of the emulsion and add it to a four-neck round bottom flask, turn on nitrogen protection, heat to 80°C while stirring, and drop the remaining 2 / 3 of the emulsion into the reaction flask within 3 hours , after all the drops were completed, the temperature was raised to 85°C, and the reaction was continued for 3 hours, then stirred and lowered to room temperature, and the discharge was filtered to obtain the target product.

Embodiment 3

[0046] Embodiment three: preparation process see figure 2 : Mix 35 grams of octamethylcyclotetrasiloxane, 10 grams of 1,3,5-trimethyl-1,3,5-tris(3,3,3-trifluoropropyl)cyclotrisiloxane, 5 grams of tetramethyltetravinyl cyclotetrasiloxane, 15 grams of methyl methacrylate, 35 grams of butyl acrylate, 4.5 grams of TX-10, 4.0 grams of fluorinated anionic emulsifier, 0.5 grams of APS, 0.7 grams of hydroxide Mix potassium and 100 grams of distilled water for 15 minutes under high shear, take out 1 / 3 of the emulsion and add it to a four-neck round bottom flask, turn on nitrogen protection, heat to 80°C while stirring, and drop the remaining 2 / 3 of the emulsion into the reaction flask within 3 hours , after all the drops were completed, the temperature was raised to 85°C, and the reaction was continued for 3 hours, then stirred and lowered to room temperature, and the discharge was filtered to obtain the target product.

[0047] Carry out electron microscope analysis to embodiment th...

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Abstract

The invention belongs to the field of modification of acrylate and in particular relates to a method for preparing fluorine-containing silicon acrylate emulsion by an emulsion polymerization method. The method comprises the following steps of: 1) mixing octamethylcyclotetrasiloxane, trifluoropropylmethyl ring trisiloxane, vinyl siloxane, an acrylate monomer, a composite emulsifier, an initiator, a pH conditioning agent and distilled water to perform pre-emulsification to obtain pre-emulsified liquid; 2) stirring part of the pre-emulsified liquid under the atmosphere of inert gas, heating at the temperature T1, adding the residual pre-emulsified liquid into a reaction system dropwise, and heating at the temperature T2; and 3) cooling to room temperature under stirring, filtering by using a 200-mesh filter screen to obtain the fluorine-containing silicon acrylate emulsion. In the preparation method, the reaction process is mild and easy to control; and the product has excellent waterproof and oilproof properties.

Description

technical field [0001] The invention belongs to the field of acrylate modification, and in particular relates to a method for preparing fluorine-silicon monomer and acrylate block copolymer emulsion by emulsion polymerization. The fluorine-containing silicon and acrylate block copolymer emulsion can be used as leather and natural fiber fabrics , Waterproof and oil-proof finishing agent for chemical fiber fabrics and paper. Background technique [0002] Polyacrylate emulsions have excellent transparency, film-forming properties, weather resistance, mechanical stability and adhesion, and are rich in raw materials and low in cost. They are widely used in coatings, textiles, leather, papermaking, adhesives and other fields. However, its stain resistance and water resistance are not ideal, and its cold resistance and heat resistance are poor, and it is prone to the phenomenon of "hot sticking and cold brittleness", which limits its further application. Fluoropolymers have prope...

Claims

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Application Information

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IPC IPC(8): C08F220/18C08F220/14C08F230/08C08F2/26C08F2/30D06M15/356D21H21/14
Inventor 陈德翔谢洪德徐磊
Owner 苏州优诺塑业有限公司
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