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Blocked quaternary ammonium group modified polysiloxane and preparation method thereof

A technology of polysiloxane and quaternary ammonium group, which is applied in the field of block quaternary ammonium group modified polysiloxane and its preparation, can solve the problems of low boiling point of isopropanol, increased production cost, low flash point, etc., and achieve the improvement of amino group content, The effect of soft performance improvement

Active Publication Date: 2020-03-17
HANGZHOU TRANSFAR FINE CHEM CO LTD +2
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AI Technical Summary

Problems solved by technology

However, there are still some defects in the block silicone oil products currently on the market: First, in the synthesis of this type of block silicone oil technology, a large amount of isopropanol or ethylene glycol monobutyl ether needs to be used as a solvent, and the boiling point of isopropanol is low, It has a low flash point, is flammable and explosive, which has buried many safety hazards in the process of production and transportation; secondly, a large amount of solvents such as isopropanol or ethylene glycol monobutyl ether exist in the finishing agent, which makes the after treatment Shade phenomenon occurs in the fabric, and the wet rubbing color fastness and dry rubbing color fastness of the fabric are reduced at the same time. If it is replaced with a high boiling point solvent, the production cost will increase significantly; Monobutyl ether) directly volatilizes into the air during the finishing heating and setting process, which significantly increases the VOC emission of the dyeing factory. Long-term inhalation or exposure to organic solvents will cause certain damage to the health of workers and surrounding residents.
The synthesis method is basically similar to the synthesis method of ordinary amino silicone oil. Strictly speaking, it still belongs to the synthesis category of amino silicone oil. Silicone oil, and the cotton fabric treated with its silicone oil emulsion has poor hydrophilicity
This reaction is an equilibrium reaction, and its synthesis conversion rate is generally about 90%. If you want to obtain low-volatile silicone oil, you need to remove low-boiling substances through high-temperature and reduced-pressure distillation in the later stage of the reaction. The energy consumption required by low boilers is quite large, and when the low volatile content is less than 1%, gelation is often prone to occur, so it is difficult to achieve the requirement that D4, D5 and D6 in silicone oil crude oil products are all less than 1000ppm, which cannot meet the EU RICH Requirements for the restriction of substances of high concern in laws and regulations

Method used

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  • Blocked quaternary ammonium group modified polysiloxane and preparation method thereof
  • Blocked quaternary ammonium group modified polysiloxane and preparation method thereof
  • Blocked quaternary ammonium group modified polysiloxane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1) Put 320g (2mol) of bis(2-dimethylaminoethyl) ether and 360g (1mol) of epoxy double head into the reaction flask with stirring and condensing device, then add 60g (1mol) of acetic acid, and start stirring , slowly raised the temperature to 95-100° C., kept the temperature for 4 hours, and then cooled to room temperature to obtain 740 g of tertiary amine-terminated silicon-containing polyether intermediate A.

[0026] 2) Weigh 148g (0.2mol) of the tertiary amino-terminated silicon-containing polyether intermediate A148g (0.2mol) prepared in the previous step, and 800g (0.2mol) of epoxy-terminated silicone oil with a molecular weight of 4000 (polymer n=50, solid content of 99.7%) , into a reaction flask equipped with a stirring and condensing device, then add 40 g (0.2 mol) of lauric acid, start stirring, slowly raise the temperature to 95-100 ° C, keep the temperature for 10 hours, cool to room temperature, and obtain 988 g of block quaternary ammonium modified Non-tox...

Embodiment 2

[0028] 1) Add 320g (2mol) of bis(2-dimethylaminoethyl) ether and 360g (1mol) of epoxy double head into the reaction flask with stirring and condensing device, then add 30g (0.5mol) of acetic acid and 100g (0.5mol) lauric acid, start stirring, slowly heat up to 100-105° C., keep warm for 5 hours, then cool to room temperature to obtain 810 g of tertiary amino-terminated silicon-containing polyether intermediate B.

[0029] 2) Weigh 1200 g (0.2 mol) of the tertiary amine-terminated silicon-containing polyether intermediate B162g (0.2 mol) prepared in the previous step, and 1200 g (0.2 mol) of epoxy-terminated silicone oil (polymer n=77, solid content 99.7%) with a molecular weight of 6000 ), added to a reaction flask with a stirring and condensing device, then added 12 g (0.2 mol) of acetic acid, started stirring, slowly raised the temperature to 95-100 ° C, kept the temperature for 12 hours, and cooled to room temperature to obtain 1374 g of block quaternary ammonium modified N...

Embodiment 3

[0031] 1) Add 320g (2mol) of bis(2-dimethylaminoethyl) ether and 360g (1mol) of epoxy double head into the reaction flask with stirring and condensing device, then add 36g (0.6mol) of acetic acid and 80g (0.4mol) lauric acid, start stirring, slowly heat up to 90-95°C, keep warm for 7 hours, cool to room temperature, and obtain 796g of tertiary amino-tertiary silicon-containing polyether intermediate C.

[0032] 2) Weigh 119.4g (0.15mol) of the tertiary amine-terminated silicon-containing polyether intermediate C119.4g (0.15mol) prepared in the previous step, and 1200g (0.15mol) of epoxy-terminated silicone oil (polymer n=104, solid content: 99.6%) with a molecular weight of 8000 mol), add it to the reaction flask with a stirring and condensing device, then add 4.5g (0.075mol) of acetic acid and 15g (0.075mol) of lauric acid, start stirring, slowly raise the temperature to 95-100°C, keep the temperature for 14 hours, and cool After reaching room temperature, 1338.9 g of block q...

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Abstract

Blocked quaternary ammonium group modified polysiloxane and a preparation method thereof are disclosed. Tertiary-amino-terminated silicon-containing polyether is synthesized; according to a similar compatibility principle, under the condition of no solvent, amino of the tertiary-amino-terminated polyether and epoxy of epoxy-terminated silicone oil can undergo homogeneous ring-opening addition, andtherefore, the synthesis technology of solvent-free (AB)n type or (ABA)n block copolymerization modified silicone oil is achieved, and introduction of siloxane into the molecular structure of the tertiary-amino-terminated polyether makes two chain ends of the chain contain amino, the amino content is obviously increased than that of existing ordinary tertiary amines, and a freely rotating silicon-oxygen bond (Si-O) is obtained. Softness of blocked quaternary ammonium group modified polysiloxane (commonly known as block silicone oil) prepared by using the tertiary-amino-terminated silicon-containing polyether as an intermediate is greatly improved.

Description

technical field [0001] The invention belongs to the field of chemical materials, and in particular relates to a block quaternary ammonium group modified polysiloxane and a preparation method thereof. Background technique [0002] With the continuous rapid economic growth and the global emphasis on environmental protection, people have put forward new expectations and requirements for the product quality of silicone softening agents. Silicone softener, as a finishing aid for textile printing and dyeing, is developing towards multi-functional, short-process and green environmental protection. At present, the three-way copolymerization technology is the mainstream new technology for the polymerization of silicone softening agents, that is, linear block polyether amino three-way copolymerization modified silicone oil, also known as (AB)n type or (ABA)n block copolymerization modified silicone oil , This type of silicone finishing agent has the characteristics of outstanding han...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08G77/452
CPCC08G77/46C08G77/452
Inventor 林云周赵婷陈天逸陈华群胡娟王胜鹏
Owner HANGZHOU TRANSFAR FINE CHEM CO LTD
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