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Preparation of carboxy silicon oil emulsion

A technology of carboxyl silicone oil and emulsion, which is applied in the field of preparation of carboxyl modified silicone oil emulsion, can solve the problems of difficult hydrolysis of siloxane, and achieve the effect of good centrifugal stability and good stability

Inactive Publication Date: 2005-05-11
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Siloxanes are insoluble in water, which makes hydrolysis of ester- or nitrile-containing siloxanes difficult and takes a long time to complete

Method used

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  • Preparation of carboxy silicon oil emulsion
  • Preparation of carboxy silicon oil emulsion
  • Preparation of carboxy silicon oil emulsion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Embodiment 1. Preparation of ester-modified silicone oil

[0043] Add 153.5 grams of 10-undecylenic acid methyl ester in 500ml four-necked bottle, heat to 80 ℃, add chloroplatinic acid catalyst (consumption is the 20ppm of total reactant amount), begin to add dropwise to system containing 50 grams of high hydrogen-containing silicone oil with a hydrogen content of 1.55%, control the dropping rate and heating rate, and keep the system temperature between 80-150°C. Removal of low boilers by pressure distillation to obtain ester-modified silicone oil modified with methyl undecanic acid. Infrared spectroscopy analysis found that at 2155cm -1 The Si-H absorption peak at has disappeared, indicating that the active hydrogen in the hydrogen-containing silicone oil has completely reacted. The product is a yellow transparent liquid with a certain viscosity, the refractive index n D 20 It is 1.4560, and η (20°C) is 152cp.

Embodiment 2

[0044] Embodiment 2. Preparation of ester-modified silicone oil

[0045] Replace methyl undecylenate with 165 grams of 10-undecylenic acid ethyl ester, repeat above-mentioned reaction, can obtain undecylenic acid ethyl ester modified ester group modified silicone oil. The product is a yellow transparent liquid with a certain viscosity, the refractive index n D 20 It is 1.4570, and η (20°C) is 160cp.

Embodiment 3

[0046] Embodiment 3. The preparation of carboxyl silicone oil emulsion

[0047] In the 500ml four-necked bottle, add 50 grams of ester-modified silicone oil in Example 2, 75 grams of octamethylcyclotetrasiloxane, 200 grams of water, 41 grams of dodecylbenzenesulfonic acid, heat up and stir and be incubated at 80 DEG C of reaction 8 hours, sampling is carried out infrared spectroscopic analysis, finds that ester group is mostly hydrolyzed (see attached figure 1 ), among them, at 1715.9cm -1 The absorption peak at is the carbonyl absorption peak in the carboxyl group, and the 1743cm -1 The absorption peak at is the carbonyl absorption peak in the unreacted ester group, at 3500-2500cm -1 A broad and weak carboxyl absorption peak appears. After the reactant was cooled, 42.4 g of 25% sodium bicarbonate aqueous solution was added, stirred at room temperature for 30 minutes, and the stirring was stopped to obtain a viscous yellowish-brown carboxy silicone oil emulsion.

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Abstract

Carboxy silicone latex emulsion is produced by: reacting the mixture of the ester group modified silicone oil, small molecular oxosilance, emulsifier, accelerating agent-dodecyl benzene sulflnic acid and water at 70-95deg.C for 5-15 hours, neutralizing by adding the sodium acid carbonate after the reactor is cooled. Its composition comprises (wt%): the use level of the ester group modified silicone oil and small molecular oxosilance is controlled by the termination product that the chain joint of organic silicon which contains carboxy has the 0.5-30% of all chain joint of organic silicon, 0.1-10% of the emolsifier, and 3-30% of the accelerating agent -dodecyl benzene sulflnic acid. It features: hydrolyzing of the ester group and polymerizing of oxosilance generate at the same time. Through the adjustment of the use level of dodecyl benzene sulflnic acid and non-ionic emolsifier, the grain size of the carboxy silicone oil latex emulsion can be modified, even the micro-latex emulsion will generate.

Description

technical field [0001] The invention relates to modified silicone oil, in particular to a method for preparing carboxy-modified silicone oil emulsion. Background technique [0002] Carboxyl-modified silicone oil is a kind of carbon-functional modified silicone oil, which means that there are carboxyl groups at both ends or side chains of the silicone molecular chain, where the carboxyl groups are connected to polysiloxane through Si-C bonds. The chemical structure is: [0003] R 1 R 2 2 SiO(SiR 2 2 O) n (SiR 2 R 3 O) m SiR 2 2 R 1 [0004] where R 1 = R 2 , R 3 or -OH,R 2 =C1~C6 organic aliphatic or aromatic substituent, R 3 =-(CH 2 ) a -COOH, n=10-10000, m=1-1000, n / m=1-1000, a=1-30. [0005] Carboxyl silicone oil has the general characteristics of silicone and the reactivity of carboxyl groups. It can be used as lubricants for fabrics, such as sewing threads, finishing agents for chemical fibers, silk and wool fabrics, bright additives for coatings, re...

Claims

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Application Information

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IPC IPC(8): C08G77/38
Inventor 张墩明蒋锡群杨昌正
Owner NANJING UNIV
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