Stable-type phosphate plasticizer and preparing method thereof

A type of phosphoric acid ester and plasticizer technology, applied in the direction of phosphorus organic compounds, etc., can solve the problems of increasing acid value, easy to return to acid, poor stability, etc., achieve good low temperature softness, solve acid return, and good cold resistance. Effect

Inactive Publication Date: 2019-05-24
天津利海石化有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the preparation process of organophosphorus flame retardants, alcohol ethers and phosphorus oxychloride are usually used as raw materials. Under acid catalysis, the crude phosphoric acid ester is obtained through esterification reaction, and finally the phosphoric acid ester after alkali washing, water washing, etc. The acid value meets the requirements, but due to its poor stability, it is particularly easy to return to acid during storage, and the acid value will gradually increase

Method used

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  • Stable-type phosphate plasticizer and preparing method thereof
  • Stable-type phosphate plasticizer and preparing method thereof
  • Stable-type phosphate plasticizer and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: in the 2000ml four-necked bottle that is equipped with heating, stirring and vacuum device, add 1020.6g

[0021] (3.15mol) diethylene glycol butyl ether and 5g (5‰) strong acid ion exchange resin Amberlyst-15, join 153.5g (1mol) phosphorus oxychloride in the constant pressure dropping funnel, open vacuum pump, form vacuum Finally, the operator opens the cooling inlet and outlet valves of the four-necked bottle glass condenser in turn, starts stirring, and controls the pressure in the four-necked bottle to 80-98Kpa. After the pressure in the four-necked bottle is stable, turn on the electric heating mantle to heat, raise the temperature to 80°C, slowly turn on the switch of the constant pressure dropping funnel, slowly add phosphorus oxychloride into the four-necked bottle, and raise the temperature to 130-135°C After equilibrating for 5 hours, after the acid value is qualified, filter out the strong acid ion exchange resin. In normal operation, the strong ...

Embodiment 2

[0022] Embodiment 2: the operating steps of embodiment 2 and embodiment 1 are basically the same, and the only difference is that alcohol ether is diethylene glycol butyl ether, and the addition of catalyst is 3‰ of alcohol ether, phosphorus oxychloride and alcohol ether The molar ratio is 1:2.5. The temperature is 110-120°C. Neutralization was carried out with 0.05% 1-butyl-2,3-dimethylimidazolium hydroxide on the dry weight of the phosphate ester. The product properties are as shown in Table 1:

Embodiment 3

[0023] Embodiment 3: the operating steps of embodiment 3 are basically the same as embodiment 1, the only difference is that the alcohol ether is dipropylene glycol butyl ether, and the addition of the catalyst is 10‰ of the alcohol ether; the catalyst is NKC-9, phosphorus oxychloride The molar ratio with alcohol ether is 1:3.5. The temperature is 140-150°C. Neutralization was carried out with 3% 1-butyl-2,3-dimethylimidazolium hydroxide on the dry weight of the phosphate ester. The traits are shown in Table 1:

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Abstract

The invention belongs to the technical field of chemical auxiliaries, and particularly relates to a stable-type phosphate plasticizer and a preparing method thereof. The preparing method comprises thefollowing steps of 1, filtering out strong-acid-type ion exchange resin after phosphorus oxychloride and alcohol ether are subjected to an esterfication reaction to obtain a crude phosphate plasticizer; 2, adding a stabilizer into the obtained crude phosphate plasticizer, wherein the addition amount of the stabilizer accounts for 0.05-3% of the dry weight of phosphate. The prepared stable-type phosphate plasticizer has high contents of oxygen and phosphorus, has flame-retardant and plasticizing effects on polyurethane rubber, cellulose, engineering plastics and the like, and has good cold tolerance, so that products are endowed with higher low-temperature softness; meanwhile, the phosphate product into which the stabilizer is added can still have the acidity smaller than 1 mg KOH / g afterbeing stored for half a year; the problem of acid reflux of the phosphate product in the storage process is solved.

Description

technical field [0001] The invention belongs to the technical field of chemical additives, in particular to a stable phosphate plasticizer and a preparation method thereof. Background technique [0002] Organophosphorus flame retardants can be used in various polymer materials. At present, the main application fields of organophosphorus flame retardants include polyurethane materials and engineering plastics. With the advancement of technology, more and more new phosphorus-based flame retardants Flame retardants have begun to appear and will be used in general-purpose plastics such as PVC and PP to gradually replace brominated flame retardants. [0003] In the preparation process of organophosphorus flame retardants, alcohol ethers and phosphorus oxychloride are usually used as raw materials. Under acid catalysis, the crude phosphoric acid ester is obtained through esterification reaction, and finally the phosphoric acid ester after alkali washing, water washing, etc. The a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/524C08K5/3445C07F9/09
Inventor 王德波姚彬
Owner 天津利海石化有限公司
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