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Macromonomer with multi-alkyl structure, preparation method and method for preparing polymer polyhydric alcohols by using macromonomer

A technology of macromonomers and polyether polyols, which is applied in the field of in-situ polymerization to prepare polymer polyols and polymer polyols, which can solve the problems of low biochemical treatment efficiency, easy generation of nitrogen oxides in incineration, high viscosity, etc.

Active Publication Date: 2017-08-25
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned method has solved the problem that the solid content of the product polymer polyol is low and the viscosity is large, all do not mention the processing problem of the decomposition product tetramethylsuccinonitrile (TMSN) of initiator azobisisobutyronitrile (AIBN) , Tetramethylsuccinonitrile is easy to sublime, highly toxic, and the efficiency of biochemical treatment is low and difficult; incineration is easy to produce nitrogen oxides, and incomplete combustion will produce highly toxic HCN

Method used

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  • Macromonomer with multi-alkyl structure, preparation method and method for preparing polymer polyhydric alcohols by using macromonomer
  • Macromonomer with multi-alkyl structure, preparation method and method for preparing polymer polyhydric alcohols by using macromonomer
  • Macromonomer with multi-alkyl structure, preparation method and method for preparing polymer polyhydric alcohols by using macromonomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] 1) Tetramethylsuccinonitrile is hydrogenated to prepare tetramethylbutanediamine:

[0078] Add 160 g of isopropanol solutions that are dissolved with 40 g of tetramethylsuccinonitrile (collected by vacuum heat exchanger), 50 g of ammonia, 0.16 g of 25% KOH aqueous solution, 10 g of Raney cobalt catalyst, and hydrogen pressure of 8 MPa in the kettle reactor , the reaction temperature is 80° C., and the stirring speed is 400 rpm for hydrogenation reaction. Then raise the temperature to 95°C, keep the pressure at 10Mpa, continue the reaction for 1h, take out the reaction solution after cooling down, remove the liquid ammonia and solvent, collect the liquid at 90-100°C under 100mbar, and weigh 30.4g.

[0079] 2) Tetramethylbutanediamine prepares tetramethylbutanediisocyanate TMBDI:

[0080]Put 400ml of chlorobenzene in a 1-liter reaction kettle, stir, blow in nitrogen to remove dissolved air, then pass in dry HCl gas and a small amount of nitrogen at a flow rate of 80L / h, ...

Embodiment 2

[0087] 1) Preparation of dimethyldiethylbutanediamine by hydrogenation of dimethyldiethylsuccinonitrile:

[0088] Referring to Example 1, the decomposition product of azobisisovaleronitrile, dimethyldiethylsuccinonitrile, was used instead of tetramethylsuccinonitrile.

[0089] 2) Dimethyldiethylbutanediamine prepares dimethyldiethylbutanediisocyanate MEBDI:

[0090] Referring to Example 1, dimethyldiethylbutanediamine was used instead of tetramethylbutanediamine.

[0091] 3) Preparation of macromolecular polyether polyol 2:

[0092] Referring to Example 1, changing the material ratio, the mass ratio of sorbitol / EO / PO is 1.84 / 14.72 / 83.44, and the measured hydroxyl number is about 34mgKOH / g.

[0093] 4) Preparation of macromonomer 2:

[0094] The dimethyl diethyl butane diisocyanate (MEBDI, 6.78g) prepared above, the bismuth isooctanoate catalyst (air chemical industry, 270mg) and hydroquinone (Rhodia, 20mg) were added in the fully mixed reaction vessel and Heat to 40°C. Th...

Embodiment 3

[0097] 1) Preparation of dimethyl diisobutyl butanediamine by hydrogenation of dimethyl diisobutyl succinonitrile:

[0098] Referring to Example 1, the decomposition product of azobisisoheptanonitrile was used to replace tetramethylsuccinonitrile with dimethyldiisobutylsuccinonitrile.

[0099] 2) Preparation of dimethyl diisobutyl butanediisocyanate MPBDI from dimethyl diisobutyl butanediamine:

[0100] Referring to Example 1, dimethyl diisobutyl butanediamine was used instead of tetramethyl butanediamine.

[0101] 3) Preparation of macromolecular polyether polyol 3:

[0102] Referring to Example 1, changing the material ratio, the mass ratio of sorbitol / EO / PO is 2.60 / 24.35 / 73.05 and about 48mgKOH / g.

[0103] 4) Preparation of macromonomer 3:

[0104] Add dimethyl diisobutyl butane diisocyanate (self-produced, MPBDI, 11.98g), tetramethylpropylenediamine catalyst (Air Chemicals, 600mg) and hydroquinone (Rhodia, 20mg) into the well-mixed The reaction vessel was heated to 60°...

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Abstract

The invention discloses a macromonomer with a multi-alkyl structure, a preparation method and a method for preparing polymer polyhydric alcohols by using the macromonomer. The basic polyether glycol is taken as a continuous phase and the macromonomer with the multi-alkyl structure is prepared into the polymer polyhydric alcohols under the effects of a chain transfer agent and a radical initiator. The initiator decomposition product can be used as the raw material for preparing the macromonomer with the multi-alkyl structure, so that the recycling of the chemical substances is realized, the use ratio of the atoms is increased, the generation of toxic and harmful waste residue is reduced and the three-waste treatment is reduced.

Description

technical field [0001] The invention relates to a macromolecular monomer with a multi-alkyl structure, a preparation method thereof, and a method for preparing polymer polyols using the macromonomer. Specifically, it relates to a method of using toxic waste in the preparation of polymer polyols to prepare macromolecular monomers, and in the presence of the macromolecular monomers as a stabilizer, in-situ polymerization in basic polyether polyols to prepare polymer polyols Alcohol method. Background technique [0002] Polymer polyol is a bulk industrial product, which can endow polyurethane products with good load-bearing properties and improve the open cell of foam. Polymer polyol is formed by in-situ polymerization of one or several vinyl monomers with basic polyether polyol as the continuous phase. The vinyl monomer used in the earliest synthesized polymer polyol is acrylonitrile. The product has low solid content and high viscosity. Under 30% solid content, it has a vis...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F220/44C08F212/08
CPCC08F290/062C08F220/44C08F212/08
Inventor 李付国鞠昌迅吴训锟杨国忠胡爽孙双翼战允庆王明永黎源
Owner WANHUA CHEM GRP CO LTD
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