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Synthesis method of special initiator for polyether polyol

A technology of polyether polyol and synthesis method, applied in the direction of chemical recovery, etc., can solve the problems of inability to obtain octyl phenolic resin, high equipment investment cost, unsuitable for industrial production, etc., and achieve control of free phenol content, low pollution, and three wastes little effect

Inactive Publication Date: 2021-07-13
南京晶典抗氧化技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although there are also some novel phenolic resin synthesis methods at present, which can reduce pollution. For example, CN107674168A provides a special microwave synthesis method. Although the method has less pollution, it is not suitable for industrial production, and the equipment investment cost is higher. Traditional method can't obtain the octyl phenolic resin of specific molecular weight of the present invention

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of synthetic method of polyether polyol special initiator, operation steps are as follows in sequence:

[0028] 1) Add 2060g of p-octylphenol, 531.5g of 37% formaldehyde solution and 20.6g of solid acid catalyst HND-6 into the reaction kettle and stir, seal the reaction kettle, raise the temperature to 60°C, pressurize by the vapor pressure of the formaldehyde solution, and keep it warm React for 3 hours, then raise the temperature to 120°C, pressurize by the vapor pressure of the formaldehyde solution, and keep it warm for 4 hours;

[0029] 2) After the reaction is finished, the catalyst is filtered out for recovery and reuse, and the filtrate is distilled and dehydrated under reduced pressure, and the dehydration temperature is less than 100°C until the anhydrous distillation is completed;

[0030] 3) Add 260g of 1800# aromatic solvent oil, keep the negative pressure below -0.08MPa, heat up to 190°C, concentrate, and remove unreacted free phenol until no free p...

Embodiment 2

[0034] A kind of synthetic method of polyether polyol special initiator, operation steps are as follows in sequence:

[0035] 1) Add 2060g of p-tertylphenol, 683.3g of 37% formaldehyde solution and 20.6g of solid acid catalyst HND-8 into the reaction kettle and stir, seal the reaction kettle, heat up to 60°C, pressurize by the vapor pressure of the formaldehyde solution itself, Heat preservation reaction for 3 hours, then raise the temperature to 120°C, pressurize by the vapor pressure of the formaldehyde solution itself, and heat preservation reaction for 4 hours;

[0036] 2) After the reaction is finished, the catalyst is filtered out for recovery and reuse, and the filtrate is distilled and dehydrated under reduced pressure, and the dehydration temperature is less than 100°C until the anhydrous distillation is completed;

[0037] 3) Add 412g of 1800# aromatic hydrocarbon solvent oil, keep the negative pressure below -0.08MPa, heat up to 190°C, concentrate, and remove unreac...

Embodiment 3

[0041] A kind of synthetic method of polyether polyol special initiator, operation steps are as follows in sequence:

[0042] 1) Add 2060g of p-octylphenol, 835.1g of 37% formaldehyde solution and 20.6g of solid acid catalyst CP002 into the reaction kettle and stir, seal the reaction kettle, raise the temperature to 60°C, pressurize with the vapor pressure of the formaldehyde solution, and keep it warm for 3 hours , and then heated up to 120°C, pressurized by the vapor pressure of the formaldehyde solution itself, and kept warm for 4 hours;

[0043] 2) After the reaction is finished, the catalyst is filtered out for recovery and reuse, and the filtrate is distilled and dehydrated under reduced pressure, and the dehydration temperature is less than 100°C until the anhydrous distillation is completed;

[0044] 3) Add 580g of 1800# aromatic hydrocarbon solvent oil, keep the negative pressure below -0.08MPa, heat up to 190°C, concentrate, remove unreacted free phenol at the same t...

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Abstract

The invention discloses a synthesis method of a special initiator for polyether polyol, wherein the initiator is essentially octyl phenolic resin. The method comprises: adding a certain amount of octyl phenol, a formaldehyde solution and a catalyst into a reaction kettle, mixing, stirring, increasing the temperature to 50-70 DEG C, carrying out a heat preservation reaction for 2-4 hours, increasing the temperature to 80-130 DEG C, carrying out a heat preservation reaction for 3-5 hours, and then carrying out filtering, distillation, concentration, preparation, and other steps to obtain the octyl phenolic resin solution. According to the invention, by adopting a closed pressurized reaction mode, the conversion rate of octylphenol is increased, and the molecular weight and molecular weight distribution of target resin can be effectively controlled; the recyclable solid acid is used for replacing the traditional strong acid, so that the requirement on production equipment is reduced, and the production process is simple, few in three wastes and low in pollution; and the high-boiling-point solvent oil is added to remove free phenol, so that the content of the free phenol can be effectively controlled, the molecular weight of the obtained octyl phenolic resin is 1100-1600, and the content of the free phenol is smaller than 0.5%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method for synthesizing a special initiator for polyether polyols. Background technique [0002] Due to its excellent performance, polyurethane foam materials are widely used in the fields of home furnishing, construction, daily necessities, transportation and home appliances. Polyether polyol is one of the key raw materials for the preparation of polyurethane foam. The polyether polyol synthesized with a specific octyl phenolic resin of a given molecular weight as an initiator has a wide range of applications and excellent performance. The key technology of polyol lies in the synthesis of initiator octyl phenolic resin. [0003] Phenolic resin polymers have a history of hundreds of years, are widely used, and their synthesis technology is very mature. However, the preparation of high-performance phenolic resins is still the key research direction of rel...

Claims

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Application Information

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IPC IPC(8): C08G8/12
CPCC08G8/12Y02P20/584
Inventor 陈福新何金义
Owner 南京晶典抗氧化技术研究院有限公司
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