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Process for producing sioc-bonded polyether siloxanes branched in the siloxane portion

A technology of siloxane and branching, applied in the field of polyether siloxane, can solve the problems of difficult product separation and unclear chemical properties, and achieve the effect of ensuring performance and quality

Pending Publication Date: 2020-12-01
EVONIK OPERATIONS GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chemical identity of the fractions II and IV thus obtained remains unclear, making it difficult to obtain defined products in this way or to isolate these products in high yields from mixtures

Method used

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  • Process for producing sioc-bonded polyether siloxanes branched in the siloxane portion

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0119] Production of cyclic branched siloxanes with a target D / T ratio of 6:1

[0120] In a 10-liter four-necked round-bottomed flask equipped with a KPG stirrer and a reflux condenser, 783 g (4.39 mol) of methyltriethoxysilane and 978.7 g (2.64 mol) of decamethylcyclopentasilane were stirred under stirring. The oxanes were heated together to 60°C and mixed with 2.98 g of trifluoromethanesulfonic acid, and the mixture was equilibrated for 4 hours. 237 g of water and 59.3 g of ethanol were then added and the batch was heated to reflux temperature for a further 2 hours. Add 159.0g of water and 978.8g (2.64mol) of decamethylcyclopentasiloxane (D 5 ), and replace the reflux condenser with a distillation bridge, and then distill off the volatile components up to 90°C in the next hour. Then 3000ml of toluene was added to the reaction batch, and the water still present in the system was removed by distillation in a water separator until the temperature of the substrate reached 100°...

Embodiment 2

[0122] Embodiment 2 (invention steps 1 and 2)

[0123] Production of acetoxy-terminated branched siloxanes

[0124] In a 500ml four-necked flask equipped with a KPG stirrer, an internal thermometer and a reflux cooler, first add 22.8g (0.223mol) of acetic anhydride and 101.2g of the DT ring produced in Example 1 under stirring (according to 29 Si-NMR spectrum D / T ratio=5.2:1, M=452.8g / mol, the proportion of SiOH / SiOEt part is 0.43mol%) and 125.9g decamethylcyclopentasiloxane (D5), then with 0.25g (0.15 ml) of trifluoromethanesulfonic acid (0.1% by mass based on the total batch) was mixed and rapidly heated to 150°C. The initially slightly cloudy reaction mixture was kept at this temperature for 6 hours with constant stirring.

[0125] After cooling of the batch, a colorless clear mobile liquid was separated, which 29 The Si-NMR spectrum showed the presence of Si-acetoxy groups in a yield of about 80% based on the acetic anhydride used, and a portion of the Si-alkoxy and SiO...

Embodiment 3

[0126] Embodiment 3 (invention step 3)

[0127] Production of branched SiOC-bonded polyether siloxanes in toluene using post-neutralization

[0128] In a 500ml four-necked flask equipped with a KPG stirrer, an internal thermometer and a reflux cooler, first add 76.1g of butane with a molar mass of 1935g / mol (molar mass is determined by OH number) in 200ml of toluene under stirring. Alcohol-started polyether alcohol (proportion 100% propylene oxide), then mixed with 20 g of the trifluoromethanesulfonic acid-treated branched acetoxysiloxane produced in Example 2. The reaction mixture was then heated to 40° C. for 1 hour with continuous stirring. The reflux cooler was then replaced with a distillation bridge with a distillate receiver, and toluene and acetic acid were removed from the batch by distillation at 70° C. with auxiliary vacuum applied.

[0129] After cooling, the distillation bottoms were mixed with 1.9 g of sodium bicarbonate, and the salt was stirred for about 30 m...

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Abstract

The present invention relates to a process for producing sioc-bonded polyether siloxanes branched in the siloxane portion. Described is a process for producing SiOC-bonded polyether siloxanes branchedin the siloxane portion from cyclic branched siloxanes of the D / T type, wherein said process comprises in a first step reacting the mixtures of cyclic branched siloxanes of the D / T type with acetic anhydride optionally in admixture with simple siloxane cycles under acid catalysis to afford acetoxy-bearing branched siloxanes, in a second step performing the equilibration of the acetoxy-modified branched siloxane with superacid, preferably with addition of acetic acid and in a third step reacting the superacid-treated acetoxysiloxane with polyetherols optionally in the presence of bases and optionally in the presence of an inert solvent.

Description

technical field [0001] The present invention relates to a process for the production of SiOC-bonded polyether siloxanes branched in the siloxane moiety. The invention additionally relates to formulations consisting of SiOC-bonded branched silicone polyethers and polyether alcohols and acetyl-terminated polyether alcohols. The invention further relates to the use of these SiOC-bonded polyether siloxanes branched in the siloxane moiety as defoamers, foam stabilizers, wetting agents, coating and flow aids and demulsifiers. Background technique [0002] "Chemie und Technologie der Silicone" by W. Noll ([Chemistry and Technology of the Silicones], Verlag Chemie GmbH, Weinheim (1960), pp. 2 ff.) is cited as relevant for describing organic polymers in this context. The terms M, D, T, Q of the structural units of the siloxane designate the relevant references. [0003] The old production methods of SiOC-bonded branched polyether siloxanes are basically based on chlorosilane chemis...

Claims

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Application Information

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IPC IPC(8): C08G77/46C09D7/65C09J11/08D06M15/647C08L83/12
CPCC08G77/46C09D7/65C09J11/08D06M15/647C08L83/12C08G77/70D06M2200/50C08G77/16C08G77/18C08G77/14C08L83/04C08L71/02C08G77/38C08G77/08C08G77/10
Inventor W·克诺特H·杜齐克
Owner EVONIK OPERATIONS GMBH
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