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Phosphate with dihydroxyl structure and preparation method thereof

A technology of bishydroxyl and phosphoric acid ester, which is applied in the field of phosphoric acid ester and its preparation, can solve the problems that affect the performance of polyurethane materials and products, and have a large impact

Inactive Publication Date: 2011-01-05
杨彦威
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the flame retardancy of polyurethane materials and products is achieved by adding organic and inorganic flame retardants, which will more or less affect the performance of polyurethane materials and products, and some have a greater impact

Method used

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  • Phosphate with dihydroxyl structure and preparation method thereof
  • Phosphate with dihydroxyl structure and preparation method thereof
  • Phosphate with dihydroxyl structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Synthesis of 1-n-butoxydiethanoloxy phosphate

[0038] 1. Product description

[0039] Product name: 1-n-butoxydiethanoloxy phosphate

[0040] Molecular Structure:

[0041]

[0042] Molecular weight: 242.11

[0043] Quality Index:

[0044] Appearance: colorless or light yellow transparent liquid

[0045] Acid value: (mgKOH / g) ≤0.02

[0046] Chromaticity: (APHA) ≤5

[0047] Boiling range: ℃ 235-240

[0048] Ignition point: ℃ 267

[0049] Lightning: °C 238

[0050] Specific gravity: (20 / 25℃) 1.017-1.023

[0051] Moisture:% ≤0.05

[0052] Physical and chemical properties:

[0053] Colorless or light yellow transparent liquid; boiling point: 236℃; refractive index: n25=1.432-1.438; solubility in water at 20℃: 25.6%; specific gravity: (20 / 25℃): 1.032-1.043; soluble in alcohol, phosphorus and other solvents .

[0054] Uses: Reactive polyurethane resin flame retardant.

[0055] 2. Synthesis technology

[0056] Raw material ratio

[0057]

[0058] 1) The first step of esterification reaction:

[0059]...

Embodiment 2

[0078] Synthesis of 1-n-butoxydipropanoloxy phosphate

[0079] 1. Product description

[0080] Product name: 1-n-butoxy dipropanol oxy phosphate

[0081] Molecular Structure:

[0082]

[0083] Molecular weight: 270.14

[0084] Quality Index:

[0085] Appearance: colorless or light yellow transparent liquid

[0086] Acid value: (mgKOH / g) ≤0.02

[0087] Chromaticity: (APHA) ≤5

[0088] Boiling range: ℃ 240-244

[0089] Ignition point: ℃ 400

[0090] Lightning: ℃ 378

[0091] Specific gravity: (20 / 25℃) 1.017-1.023

[0092] Moisture:% ≤0.05

[0093] Physical and chemical properties:

[0094] Colorless or light yellow transparent liquid; boiling point: 236℃; refractive index: n25=1.432-1.438; solubility in water at 20℃: 25.6%; specific gravity: (20 / 25℃): 1.032-1.043; soluble in alcohol, phosphorus and other solvents .

[0095] use:

[0096] Polyurethane resin flame retardant.

[0097] 2. Synthesis technology

[0098] Raw material ratio

[0099]

[0100] 1) The first step of esterification reaction:

[0101...

Embodiment 3

[0121] Synthesis of 1-n-Butoxy Diethylene Glycoloxy Phosphate

[0122] 1. Product description

[0123] Product name: 1-n-butoxy diethylene glycol oxy phosphate

[0124] Molecular Structure:

[0125]

[0126] Molecular weight: 330.11

[0127] Quality Index:

[0128] Appearance: colorless or light yellow transparent liquid

[0129] Acid value: (mgKOH / g) ≤0.02

[0130] Chroma: (APHA) ≤8

[0131] Boiling range: ℃ 255-260

[0132] Ignition point: ℃ 247

[0133] Lightning: °C 228

[0134] Specific gravity: (20 / 25℃) 1.019-1.026

[0135] Moisture:% ≤0.05

[0136] Physical and chemical properties:

[0137] Colorless or light yellow transparent liquid; boiling point: 236℃; refractive index: n25=1.448-1.455; solubility in water at 20℃: 48.6%; specific gravity: (20 / 25℃): 1.042-1.049, soluble in alcohol, phosphorus and other solvents .

[0138] use:

[0139] Reactive polyurethane resin flame retardant.

[0140] 2. Synthesis technology

[0141] Raw material ratio

[0142]

[0143] 1) The first step of esterificati...

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Abstract

The invention discloses phosphate with a dihydroxyl structure and a preparation method thereof. The molecular structure general formula of the phosphate is CH3(CH2)nOPO(O(CH2)mOH)2 or CH3(CH2)nOPO(O(CH2)mO(CH2)m)OH)2, wherein n is not less than 3, and m is not less than 2. The preparation method of the phosphate comprises the following steps of: (1) first-step esterification for the first time; (2) esterification for the second time; (3) alkali washing and water washing; (4) dealcoholization and water washing; and (5) thin film evaporation-molecular distillation and purification. The phosphate prepared by adopting the preparation method has the purity up to more than 99.9 percent, is mainly used as a chain extender of polyurethane series products and endows the polyurethane series products (reactive-type polyurethane flame retardant) with excellent flame retardation property.

Description

Technical field [0001] The invention relates to a phosphoric acid ester with a double hydroxyl structure and a preparation method thereof; it belongs to the field of organic synthesis. Background technique [0002] Phosphate ester as a non-toxic flame retardant has a wide range of applications in plastics, rubber, polymer resins and other fields, and is more and more popular. Basically replace the halogen flame retardant. However, in the polyurethane industry, phosphate esters currently on the market do not have hydroxyl or amino groups that can react with isocyanates and are restricted. [0003] Coatings produced with polyurethane have excellent mechanical properties, outstanding chemical stability and excellent weather resistance. They are widely used in high-end applications such as automobiles, luxury buses, high-speed trains, airplanes, wood furniture, architectural exterior wall coatings, household appliances, etc. field. The elastomer produced by polyurethane is colorless...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
Inventor 杨彦威
Owner 杨彦威
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