Preparation method of bio-based pentamethylene diisocyanate trimer

A technology based on pentamethylene diisocyanate and pentamethylene diisocyanate, applied in the field of preparation of bio-based pentamethylene diisocyanate trimer, can solve the influence of trimer stability, catalyst concentration sensitivity, three The viscosity of the polymer increases and other problems, so as to reduce the preparation cost, make the color transparent, and improve the bending resistance.

Active Publication Date: 2019-08-30
CNOOC CHANGZHOU PAINT & COATINGS IND RES INST +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But it still has some deficiencies in the process of synthesizing the trimer: 1) as a bio-based raw material, its monomer contains more impurities, if these impurities are not removed in the process of synthesizing the trimer, the trimer Stability will be affected; 2) Since the reactivity of pentamethylene diisocyanate is higher than that of hexamethylene diisocyanate, it is more sensitive to the concentration of catalyst in the process of synthesizing trimer, and excessive catalyst will cause trimerization Viscosity increases, chroma increases, and even implosion occurs; 3) The removal of residual single after reaction and the performance of trimer need to be balanced

Method used

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  • Preparation method of bio-based pentamethylene diisocyanate trimer

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Embodiment 1

[0035] The preparation method of the bio-based pentamethylene diisocyanate trimer of the present embodiment comprises the following steps:

[0036] 1) Take the crude product of pentamethylene diisocyanate monomer (PDI) (Gansu Yinguang) and carry out inert atmosphere purging, the purity of the crude product of PDI is ≥ 98%, the mass fraction of isocyanate is ≥ 50%, the chromaticity ≤ APHA40, insoluble ≤1wt%, specifically: get 300 parts by mass of PDI crude product, add 0.5 parts by mass of tri(dodecyl) phosphite, shake to fully disperse, then pass into nitrogen purging, the flow rate of purging gas is 40ml / min, the purging temperature is 220°C, and the purging time is 2h. After purging, take out the PDI sample and carry out distillation operation. The temperature at the bottom of the distillation tower is 180°C, and the distillation time is 1h. The light fraction is collected as PDI For the fine product, add 0.2 parts by mass of tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)pro...

Embodiment 2

[0041] The preparation method of the bio-based pentamethylene diisocyanate trimer of the present embodiment comprises the following steps:

[0042] 1) Take the PDI crude product and carry out inert atmosphere purging, specifically: take 300 mass parts of the PDI crude product, add 0.5 mass parts of tris(dodecyl) phosphite, shake to fully disperse, and then pass nitrogen gas to purify , the flow rate of the purge gas is 55ml / min, the purge temperature is 230°C, and the purge time is 2h. The monomer is distilled off, the distillation is stopped, and the PDI fine product is obtained, and 0.2 parts by mass of tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid]pentaerythyl ester is added for stable storage. use;

[0043] 2) Take 300 parts by mass of PDI high-quality goods, add 0.2 parts by mass of antioxidant tetrakis [3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentapentyl alcohol ester, add catalyst A three (2 , 0.2 parts by mass of 4-di-tert-butylphenyl)phosphi...

Embodiment 3

[0046] The preparation method of the bio-based pentamethylene diisocyanate trimer of the present embodiment comprises the following steps:

[0047] 1) Take the PDI crude product and carry out inert atmosphere purging, specifically: take 300 mass parts of the PDI crude product, add 2 mass parts of tris (dodecyl) phosphite, shake to fully disperse, pass into nitrogen purging, The flow rate of the purge gas is 40ml / min, the purge temperature is 220°C, and the purge time is 1h. After the purge is completed, the PDI sample is taken out and subjected to vacuum distillation. The distillation temperature is 165°C, and the distillation pressure is 15mbar. The monomer was distilled out, and after the monomer was taken out, the vacuum distillation was carried out again. The above-mentioned vacuum distillation was repeated 3 times, and the vacuum distillation operation was stopped to obtain the fine PDI. Add 0.2 parts by mass of tetrakis [3-(3,5-di tert-butyl-4-hydroxyphenyl) propionate] ...

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Abstract

The invention relates to the technical field of preparation of polyisocyanates, and in particular relates to a preparation method of a bio-based pentamethylene diisocyanate trimer. The preparation method of the bio-based pentamethylene diisocyanate trimer comprises the following steps: 1) performing purification treatment on a crude pentamethylene diisocyanate monomer; and 2) mixing the purified pentamethylene diisocyanate monomer, an antioxidant and a catalyst A, performing a reaction at 50-150 DEG C for 0.5-10 h, adding a catalyst B, performing a reaction at 50-160 DEG C for 0.2-10 h, addinga terminating agent to terminate the reaction, and removing pentamethylene diisocyanate monomer in reaction products to obtain the bio-based pentamethylene diisocyanate trimer.

Description

technical field [0001] The invention relates to the technical field of polyisocyanate preparation, in particular to a preparation method of bio-based pentamethylene diisocyanate trimer. Background technique [0002] Polyisocyanates are mainly used as curing agents for two-component polyurethanes. In the field of polyurethane, the commonly used polyisocyanate curing agents are diphenylmethane diisocyanate (MDI), toluene diisocyanate (TDI), polydiphenylmethane diisocyanate (pMDI), hexamethylene diisocyanate (HDI) and Isophorone diisocyanate (IPDI), etc., these curing agents are all derived from petroleum, and will be affected by the supply and demand of petroleum resources during use. Based on the short-term non-renewability of petroleum resources and the sustainable development of materials, it is urgent to develop bio-based polyisocyanates to enrich the selection of curing agents for polyurethane. As aromatic curing agents, MDI and TDI have the advantages of strong reactiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/34C09D175/04C09D5/08C08G18/79
CPCC07D251/34C08G18/792C09D5/08C09D175/04
Inventor 谭伟民雒新亮狄志刚史立平刘仲阳郁飞何毅
Owner CNOOC CHANGZHOU PAINT & COATINGS IND RES INST
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