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Preparation method of pyrophosphate piperazine

A technology for piperazine pyrophosphate and piperazine, which is applied in the field of chemistry, can solve the problems of slow salt formation between phosphoric acid and piperazine, increase production cost, increase transportation cost and other problems, and achieves low price, reduced raw material cost and stable properties. Effect

Active Publication Date: 2016-10-12
寿光普尔化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the following disadvantages: (1) Since phosphoric acid is a medium-strong acid, the speed of salt formation between phosphoric acid and piperazine is relatively slow, and it generally takes a long time or needs to reduce the temperature to generate precipitates; (2) The reaction system belongs to an acidic environment. In the process of removing solvent water, heating will aggravate the corrosion of the acidic system to the equipment; (3) the acidic dehydration environment makes some piperazine groups undergo intermolecular dehydration side reactions, and the product color is yellowish or even grayish brown etc., and the use of inert gas protection will undoubtedly increase production costs; (4) Phosphoric acid or concentrated phosphoric acid, one of the raw materials, is usually in a liquid state, and requires special equipment and protective measures during transportation, and storage also needs to be considered in large quantities. Uncertainty to production, increased transportation costs

Method used

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  • Preparation method of pyrophosphate piperazine
  • Preparation method of pyrophosphate piperazine
  • Preparation method of pyrophosphate piperazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a 10L glass reaction kettle equipped with a stirrer, a thermometer and an exhaust pipe, add 1.15kg of ammonium dihydrogen phosphate and 1000mL of distilled water, raise the temperature to 85-90°C, add 430g of anhydrous piperazine solids in batches, and keep the temperature for 3 hours. A white turbid liquid intermediate was obtained; 6 L of liquid paraffin was added, stirred and reacted at 210° C. for 1 hour, filtered, the precipitate was washed with petroleum ether, and dried to obtain a white powder of piperazine pyrophosphate.

[0025] According to the literature, the solid insoluble matter obtained at 80°C is mainly piperazine hydrogen phosphate, the solid insoluble matter obtained at 150°C is mainly a mixture of piperazine hydrogen phosphate and piperazine pyrophosphate, and at 210°C is pyrophosphate piperazine phosphate.

Embodiment 2

[0027] In a 10L vacuum kneader, add 2.35kg of ammonium dihydrogen phosphate and 1.5L of distilled water, raise the temperature to 85-90°C, add 860g of anhydrous piperazine solid in batches, keep the reaction for 1 hour, and remove water under vacuum for 1 hour. Under vacuum and reduced pressure, the reaction temperature was gradually increased to 230° C., and the kneading reaction was continued for 40 minutes to obtain a white powder of piperazine pyrophosphate.

[0028] Embodiment 2 technology and comparative example technology cost accounting table (cost saving 14.4%)

[0029]

Embodiment 3

[0031] Add 1.15kg ammonium dihydrogen phosphate and 1.1L distilled water to a 10L glass reactor equipped with a stirrer, a thermometer and an exhaust pipe, raise the temperature to 85-90°C, add 430g of anhydrous piperazine solids in batches, and keep the temperature for 3 hours. , to obtain a white turbid liquid intermediate; add 7L of high-temperature silicone oil, stir and react at 220°C for 1 hour, filter, wash the precipitate with petroleum ether, and dry to obtain a white powder of piperazine pyrophosphate. From figure 2 It can be seen that the product has high thermal stability, and the 5% decomposition temperature is 299°C

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Abstract

The invention discloses a preparation method of pyrophosphate piperazine. The preparation method comprises the following steps: mixing ammonium dihydrogen phosphate and piperazine in an aqueous solution according to a mole ratio of 2:1, heating to remove ammonia, and dewatering for condensation to obtain the pyrophosphate piperazine. According to the preparation method, the shortcomings that conventional liquid phosphoric acid serving as a phosphorous source is difficult to transport and store are overcome; a reaction system is a weak-alkaline environment, so that erosion of the phosphoric acid serving as the phosphorous source to equipment is avoided; ammonia released during reaction can be used as protection atmosphere of the reaction system, and the whiteness value of a product meets the market requirement. Compared with a phosphoric acid-piperazine method, the preparation method has the advantage of saving the raw material cost by 10 to 15 percent.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a preparation method of piperazine pyrophosphate. Background technique [0002] As a phosphorus-nitrogen-containing halogen-free flame retardant, piperazine pyrophosphate has attracted great attention from domestic and foreign manufacturers because of its excellent flame-retardant performance. It is a new type of halogen-free flame retardant with great market potential. Generally speaking, piperazine pyrophosphate has the following advantages: (1) The size of piperazine cation and hydrogen pyrophosphate in piperazine pyrophosphate is large, and the charge density is extremely low, which is in line with the combination of large anion and large cation in the chemical principle (2) pyrophosphate is bonded to the nitrogen atom in piperazine when heated to form a P-N bond with a bond energy exceeding 600kJ / mol, thus making the carbon atom in piperazine partly fast Carbonization, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/027C07D295/023
CPCC07D295/023C07D295/027
Inventor 窦伟刘伟生孙诗豪张国林唐晓亮
Owner 寿光普尔化工有限公司
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