Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Fine-grained polypiperazine phosphate flame retardant as well as preparation method and application thereof

A polyphosphoric acid, fine-grained technology, applied in the field of flame retardants, can solve the problems of reducing the mechanical properties or processing properties of flame-retardant polymer materials, piperazine polyphosphate cannot be directly used in flame-retardant polymer materials, and poor dispersibility, etc., to achieve Achieve the effect of solvent recycling, low cost and avoid yellowing

Pending Publication Date: 2020-10-16
HUBEI INST OF AEROSPACE CHEMOTECH +1
View PDF5 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The particle size and particle size distribution of piperazine polyphosphate are an important technical index affecting its performance; as an inorganic additive flame retardant, there is a large difference in properties between piperazine polyphosphate and the matrix of organic polymer materials. Poor performance; piperazine polyphosphate with large particle size is blended into the matrix, which will reduce the mechanical properties or processing properties of flame-retardant polymer materials
The particle size of the piperazine polyphosphate flame retardant prepared in the prior art is relatively coarse. At present, in order to promote the dispersion of piperazine polyphosphate, improve its compatibility with polymer materials, and improve the flame retardant performance, it is necessary to make the prepared coarse piperazine The particle size of piperazine polyphosphate is further fine-grained, that is, it can be used for flame-retardant polymer materials after being pulverized. The process is cumbersome, the cost is high, and the prepared piperazine polyphosphate cannot be directly used for flame-retardant polymer materials. defect

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Fine-grained polypiperazine phosphate flame retardant as well as preparation method and application thereof
  • Fine-grained polypiperazine phosphate flame retardant as well as preparation method and application thereof
  • Fine-grained polypiperazine phosphate flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 338g of acetic acid (industrial grade) and 22.5g of piperazine into a 500ml three-necked flask, raise the temperature to 80°C and add 59.0g of polyphosphoric acid, react at 100°C for 8 hours, stop heating, cool to room temperature, filter, and dry to obtain 67.3g fine-grained piperazine polyphosphate flame retardant, yield 82.5%.

[0041] The particle size of the prepared fine-grained piperazine polyphosphate flame retardant was detected by a laser particle size analyzer. The test results are shown in Table 1. The product particle size D50 is 18.2 μm, and the particle size of the fine-grained piperazine polyphosphate flame retardant distributed as figure 2 Shown; its thermal decomposition temperature is as image 3 shown, from image 3 It can be concluded that the 5% initial decomposition temperature of the fine-grained piperazine polyphosphate flame retardant is higher than 300°C, and has good flame retardancy.

[0042] The whiteness of the prepared fine-graine...

Embodiment 2

[0046] Add 155g of recovered acetic acid filtrate and 25.75g of piperazine to a 500ml three-necked flask, heat up to 70°C and add 25.30g of polyphosphoric acid, react at 105°C for 6 hours, stop heating, cool to room temperature, filter, and dry to obtain 47.1g Fine-grained piperazine polyphosphate flame retardant with a yield of 92.3%.

[0047] The particle size of the prepared fine-grained piperazine polyphosphate flame retardant was detected by a laser particle size analyzer. The test results are shown in Table 2. The product particle size D50 is 17.7 μm, and the particle size of the fine-grained piperazine polyphosphate flame retardant distributed as Figure 4 Shown; its thermal decomposition temperature is as Figure 5 shown, from Figure 5 It can be concluded that the 5% initial decomposition temperature of the fine-grained piperazine polyphosphate flame retardant is higher than 300°C, and has good flame retardancy.

[0048] The whiteness of the prepared fine-grained p...

Embodiment 3

[0052]Add 230g of acetic acid (industrial grade) and 22.6g of piperazine into a 500ml three-necked flask, raise the temperature to 77°C and add 34.7g of polyphosphoric acid, react the resulting mixture at 110°C for 4 hours, stop heating, cool to room temperature, filter, and dry to obtain 48.7g fine-grained piperazine polyphosphate flame retardant, yield 85.0%.

[0053] The particle size of the prepared fine-grained piperazine polyphosphate flame retardant was detected by a laser particle size analyzer. The test results are shown in Table 3. The product particle size D50 is 13.2 μm, and the particle size of the fine-grained piperazine polyphosphate flame retardant distributed as Figure 6 Shown; its thermal decomposition temperature is as Figure 7 shown, from Figure 7 It can be concluded that the 5% initial decomposition temperature of the fine-grained piperazine polyphosphate flame retardant is higher than 300°C, and has good flame retardancy.

[0054] The whiteness of t...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Particle sizeaaaaaaaaaa
Particle sizeaaaaaaaaaa
Solution temperatureaaaaaaaaaa
Login to View More

Abstract

The invention discloses a fine-grained polypiperazine phosphate flame retardant. The particle size D50 of the fine-grained polypiperazine phosphate flame retardant is less than 20 [mu]m. The inventionalso discloses a preparation method of the fine-grained polypiperazine phosphate flame retardant. The preparation method comprises the following steps: adding acetic acid into a reaction device, adding piperazine under stirring, heating; adding polyphosphoric acid, stirring, reacting at 100-110 DEG C; cooling to the room temperature, filtering, and drying to obtain the fine-grained polypiperazinephosphate flame retardant. The method can be used for directly preparing the polypiperazine phosphate flame retardant with a small particle size, the product can be used without a crushing procedureafter being dried, and the acetic acid filtrate obtained by filtering after reaction can be directly used for the next reaction without treatment.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a fine-grained piperazine polyphosphate flame retardant and its preparation method and application. Background technique [0002] With the rapid development of China's economy, the consumption of flame retardants has increased significantly. Piperazine phosphate (piperazine polyphosphate) flame retardants are halogen-free, low smoke, low toxicity, good thermal stability, and excellent flame retardant performance. And other characteristics, in line with the requirements of green chemistry, has developed rapidly in recent years. [0003] At present, polyphosphoric acid and piperazine have been used as raw materials to prepare piperazine polyphosphate with a phosphoric acid unit length of 2.2-10, and its particle size (D50) is less than 30 μm. The reaction can be carried out in solvents such as alcohols, aromatic alkanes, and halogenated alkanes. Carried out; by directly u...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C08K5/3462C07D295/027C07D295/023
CPCC07D295/023C07D295/027C08K5/3462C08K2201/005
Inventor 金凤常智俐田志雄孟喜叶丹阳李俊彬姚小龙何伟谌能办李凤宇
Owner HUBEI INST OF AEROSPACE CHEMOTECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com