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Method for preparing high-purity and high-yield pyrophosphoric acid piperazine and application thereof

A high-purity technology of piperazine pyrophosphate, applied in the field of preparation of piperazine pyrophosphate, can solve problems such as high price of raw materials, inability to be widely used, insufficient performance of finished products, etc., and achieves avoiding the interference of sodium ions, avoiding incomplete risks, Responsive effect

Active Publication Date: 2016-05-04
ZHONGSHAN COMPLORD NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods for preparing piperazine pyrophosphate have disadvantages to varying degrees, resulting in insufficient performance and high cost of the finished product, which cannot be widely used
[0009] Using the first method, after the product is obtained, wash with water to remove the by-products. In fact, even by washing with water, the sodium chloride and sodium piperazine pyrophosphate produced by the side reaction cannot be completely removed.
In general, if alkaline substances remain in the system, it may cause adverse effects if the piperazine pyrophosphate is used in semiconductors, electronic equipment, etc.
In addition, the yield rate of this method is about 53%, the yield rate is low, and the price of raw materials is high, waste treatment needs factors such as cost, it is difficult to cheaply manufacture piperazine pyrophosphate as the target
[0010] Adopt second kind of method, need to react by phosphoric acid and piperazine earlier, and adopt suitable solvent (as alcohol solvent), piperazine diphosphate is precipitated out, then the piperazine diphosphate that precipitates out is added to high boiling point solvent ( Such as in IP2028), and adding an appropriate amount of catalyst for dehydration condensation reaction, thereby obtaining the target piperazine pyrophosphate; this method needs to use a solvent to precipitate piperazine diphosphate when synthesizing piperazine diphosphate, and the solvent recovery used is compared Troublesome, high cost; and also need a solvent as a medium for dehydration during condensation, the solvent used is more expensive, recyclable but has a large loss, and at the same time the product after solvent treatment is greasy and needs further purification treatment, cost High and cumbersome to operate; after adding a certain amount of catalyst to condense into a product, without purification treatment, it may contain impurities such as acidic substances or salts, which will affect the quality of the product, and at the same time, the product will turn yellow after high temperature treatment risks of

Method used

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  • Method for preparing high-purity and high-yield pyrophosphoric acid piperazine and application thereof
  • Method for preparing high-purity and high-yield pyrophosphoric acid piperazine and application thereof
  • Method for preparing high-purity and high-yield pyrophosphoric acid piperazine and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] In a 100L reactor with a stirring and refluxing device, add 11.55kg of phosphorus pentoxide, add 9.38kg of 85% phosphoric acid dropwise while stirring, and after the dropwise addition is completed, the temperature of the reactor is controlled to 200±5°C, and this temperature is maintained for 1h .

[0049] Then cool down to 80±5℃, add 63kg of glacial acetic acid to the reaction kettle, after stirring for 0.5h, add anhydrous piperazine in batches, add a total of 10.5kg, after adding, maintain the reflux state of the reaction solution and keep the temperature at 115 -120℃, time 2h.

[0050] After that, it was cooled to room temperature and filtered until no obvious liquid dripped. The filter cake was put into a vacuum rake dryer. The temperature of the heat transfer oil was set at 185±5℃, the vacuum degree was kept at 0.05±0.02Mpa, and the drying time was 3h. smash.

[0051] 31.10kg of product can be obtained, yield 96.49%, purity 99.2%, moisture 0.1%, whiteness 94%, pa...

Embodiment 2

[0053] In a 500L reaction kettle with stirring and reflux device, add 56.83kg of phosphorus pentoxide, add 46.15kg of 85% phosphoric acid dropwise while stirring, and dropwise add to it. h.

[0054] Then the temperature was lowered to 80±5°C, 310kg of glacial acetic acid was added to the reaction kettle, and after stirring for 0.5h, anhydrous piperazine was added in batches, and a total of 52.1kg was added. -120℃, time 3h.

[0055] After that, it was cooled to room temperature, filtered until no obvious liquid dripped, and the filter cake was put into a vacuum rake dryer. machine crushing.

[0056] 151.50kg of product can be obtained, yield 95.52%, purity 99.1%, moisture 0.1%, whiteness 95%, particle size D 50 = 8.14 μm, D 98 =18.38μm, high-purity piperazine pyrophosphate with initial decomposition temperature ≥280°C.

Embodiment 3

[0058] In the 1000L reactor with stirring and refluxing device, add 113.66kg of phosphorus pentoxide, add 92.3kg of 85% phosphoric acid dropwise while stirring, and dropwise add to control the temperature of the reactor at 202±5°C, keeping this temperature at 1.5 h.

[0059] Then cool down to 80±5℃, add 600kg of glacial acetic acid to the reaction kettle, after stirring for 0.5h, add anhydrous piperazine in batches, add 104.2kg in total, after adding, maintain the reflux state of the reaction solution, keep the temperature at 116 ~120℃, time 3.5h.

[0060] Then cool down to room temperature, filter by pressure until no obvious liquid drips, put the filter cake into the vacuum rake dryer, set the temperature of the heat transfer oil to 188±5℃, keep the vacuum degree at 0.05±0.03Mpa, and the drying time is 4h. The product uses a jet mill. smash.

[0061] 301.68kg of product can be obtained, yield 95.10%, purity 99.2%, moisture 0.1%, whiteness 94%, particle size D 50 = 8.12 μm...

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Abstract

The invention discloses a method for preparing high-purity and high-yield pyrophosphoric acid piperazine. Phosphorus pentoxide is added into a reaction still which is provided with a stirring and recycling device, stirring is conducted while 85% phosphoric acid is added in a dropwise mode, and after dropping is finished, the temperature of the reaction still is adjusted to 150-250 DEG C and kept for 0.5-5 h through the temperature rising control of the reaction still; the temperature of the reaction still is reduced to 50-100 DEG C through the temperature decreasing control of the reaction still, and glacial acetic acid is added into the reaction still and stirred for 0.1-2 h; piperazine is added in batches, and the temperature of the reaction still is kept between 80 DEG C and 150 DEG C for 1-5 h; the temperature is decreased to the indoor temperature, filter pressing is conducted, filter cakes are dried through a rake type drier, a clamping sleeve of the rake type drier is heated by heat transfer oil, the temperature of the heat transfer oil of the clamping sleeve of the rake type drier is controlled between 100 DEG C and 250 DEG C, the vacuum degree is 0.01-0.1 Mpa, a vacuum desolventizzazione is kept for 1-6 h, and then high-purity pyrophosphoric acid piperazine crystals are prepared. The purity of the product prepared through the method is 99% or above, the yield of the product prepared through the method is 95% or above, the whiteness of the product prepared through the method is 93% or above, the heat stability of the prepared pyrophosphoric acid piperazine is good, no byproduct is produced, and cost is low.

Description

technical field [0001] The invention relates to the preparation field of piperazine pyrophosphate, in particular to a method for preparing piperazine pyrophosphate with high purity and high yield and application thereof. Background technique [0002] Piperazine pyrophosphate has excellent flame retardant effect. It is an important component of halogen-free additive flame retardants and is increasingly used in the flame retardant industry. Therefore, how to achieve high purity and high yield? The efficient preparation of piperazine pyrophosphate is a constant concern in the flame retardant industry. [0003] At present, the preparation method of various piperazine pyrophosphate has been disclosed, for example: [0004] Japanese Patent Laid-Open No. 47-8891 discloses a method in which piperazine hydrochloride and sodium pyrophosphate are reacted in an aqueous solution to obtain piperazine pyrophosphate as a precipitate which is hardly soluble in water. [0005] The specifica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/023C07D295/027C08L23/12C08K5/00C08K5/52
CPCC07D295/023C07D295/027C08L23/12C08L2201/02C08L2201/22C08L2205/02C08L23/06C08K5/00C08K5/5205
Inventor 张秀芹梁顺全何燕岭
Owner ZHONGSHAN COMPLORD NEW MATERIALS CO LTD
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